The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H...The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H2O](bdc)}n which has been characterized by single- crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group P2/n with a = 7.0001(2), b = 11.5540(3), c = 11.4192(1) ? = 101.754(2)? V = 904.21(4) 3, Z = 2, C18H20MnN2O8, Mr = 447.30, Dc = 1.643 g/cm3, F(000) = 462 and m(MoK? = 0.783 mm-1. The final R and wR are 0.0499 and 0.1301, respectively for 1335 observed reflections with I ≥ 2(I). The Mn (Ⅱ) is six-coordinated in a distorted octahedral geometry. 4,4?Bipyridine in a m-bridge mode links [Mn(H2O)4]2+ into a linear cation chain. bdc acts as a counter anion and links the linear chains into a three-dimensional structure through hydrogen bonds.展开更多
A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·2C3H7OH·2H2O 1 (abo = R(-)-2-amino-1-butanol) has been synthesized from VO2^+ in organic solvents and its crystal structure was rep...A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·2C3H7OH·2H2O 1 (abo = R(-)-2-amino-1-butanol) has been synthesized from VO2^+ in organic solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a = 11.419(9), b = 16.811(16), c = 15.521(12) A, β= 102.98(2)°, V= 2903(4) A^3, Z = 4, C15H46N3O19V5, Mr = 827.25, Dc = 1.893 g/cm^3, 2(MoKα) = 0.71073 A, μ = 1.636 mm^-1, F(000) = 1696, the final R = 0.0696 and wR = 0.1361 for 4641 observed reflections with I 〉 2σ(I). The compound is based on decavanadate clusters [V10O28]^6-. The hydrogen bonding interactions among Habo^+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.展开更多
A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and d...A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490(15), b = 7.0847(16), c = 30.845(3)A, β= 95.33(3)°, V = 1599.0(5)A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F(000) = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones (I 〉2σ(I)). In the crystal structure, mononuclear units [Cu(naphdien)]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.展开更多
Two zinc(Ⅱ) compounds, [Zn(L)(H2O)2]n 1 and [Zn(4,4'-bpy)(H2O)4](L) 2 (H2L = trans,trans-1,3 butadiene 1,4-dicarboxylic acid), were synthesized by hydrothermal methods and characterized by single-cryst...Two zinc(Ⅱ) compounds, [Zn(L)(H2O)2]n 1 and [Zn(4,4'-bpy)(H2O)4](L) 2 (H2L = trans,trans-1,3 butadiene 1,4-dicarboxylic acid), were synthesized by hydrothermal methods and characterized by single-crystal X-ray diffraction analyses. Compound 1 crystallizes in monoclinic, space group C2/c with a=15.4970(16), b = 5.4976(6), c = 10.7113(12) A, β=96.298(6)°, C6H8O6Zn, Mr = 241.50, V = 907.06(17) A^3, Z = 4, D, = 1.768 g/cm^3, F(000) = 488,μ = 2.703 mm^-1, S = 1.060, the final R = 0.0256 and wR = 0.0660 for 968 observed reflections with Ⅰ 〉 2σ(Ⅰ). Compound 2 crystallizes in triclinic, space group P1^- with a = 6.915(2), b = 7.166(2), c = 10.363(3) A, α = 73.250(4), β = 84.429(4), γ = 61.605(3)°, C16H2ON2O8Zn, Mr = 433.70, V = 432.1 (2) A^3, Z = 1, D, = 1.667 g/cm^3, F(000) = 224 and μ= 1.471 mm^-1, S = 1.118, the final R = 0.0486 and wR = 0.1077 for 1352 observed reflections with Ⅰ〉 2σ(Ⅰ). Upon using the assembly strategy of combination of coordination polymer chains with intermolecular hydrogen bonds, three-dimensional frameworks of complexes 1 and 2 were formed.展开更多
The supramolecular compound [(AgI3)(4-HBPFA)2(H2O)] (Mr = 1361.11) was synthesized via the reaction of 1,1?-bis[(4-pyridylamino)carbonyl]ferrocene (4-BPFA) with AgI, and structurally characterized by single-crystal X-...The supramolecular compound [(AgI3)(4-HBPFA)2(H2O)] (Mr = 1361.11) was synthesized via the reaction of 1,1?-bis[(4-pyridylamino)carbonyl]ferrocene (4-BPFA) with AgI, and structurally characterized by single-crystal X-ray diffraction analysis. Crystal data: monoclinic, space group C2/c, a = 1.6783(3), b = 10.646(2), c = 2.5419(5) ?, β = 93.66(3)o, V = 4532.2(16) ?3, Z = 4, Dc = 1.995 g/cm3, F(000) = 2632 and μ = 3.158 mm-1. The compound consists of (4- HBPFA)+, (AgI3)2- and H2O. In the structure, the adjacent (4-HBPFA)+ are linked by C–H…O and N–H…N hydrogen bonds into 1-D chains which are further linked by C–H…I and N–H…I hydrogen bonds as well as intermolecular π-π stacking interactions to form a 3-D supramolecular compound.展开更多
The title compound, {[Cu(2,2?-bipy)(C7H4O5S)(H2O)2]?H2O}n (2,2?-bipy = 2,2?- bipyridine), was synthesized by the hydrothermal reaction of Cu(NO3)2?3H2O, 2,2?-bipyridine and 2-sulphobenzoic acid, and structurally cha...The title compound, {[Cu(2,2?-bipy)(C7H4O5S)(H2O)2]?H2O}n (2,2?-bipy = 2,2?- bipyridine), was synthesized by the hydrothermal reaction of Cu(NO3)2?3H2O, 2,2?-bipyridine and 2-sulphobenzoic acid, and structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a = 9.21(3), b = 10.17(3), c = 10.77(3) ?, α = 77.017(16), β = 89.80(8), γ = 68.46(7)°, V = 911(5) ?3, Z = 2, (D/s)max= 0.001, Mr = 473.94, Dc = 1.728 g/cm3, μ(MoKα) = 1.365 mm-1, F(000) = 486, the final R = 0.0246 and wR = 0.0628 for 3809 observed reflections with I > 2σ(I). The mononuclear crystal structure extends into a two-dimensional net- work via hydrogen-bonding interactions and a three-dimensional framework is further formed by means of π-π stacking interactions.展开更多
A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure...A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5)A, a = 101.5310(10), β = 90.2610(10), γ = 116.4600( 10)% V = 1459.44(8)A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D'…A' H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between (tataH)^+, [Mn(pydc)2]^2- and crystal water.展开更多
A new copper(Ⅱ) complex [Cu(PDA)(H 2O) 2] was synthesized and its structure was determined. Cu(Ⅱ) is five coordinated in a tetragonal pyramid geometry. The two coordinating water molecules are different and t...A new copper(Ⅱ) complex [Cu(PDA)(H 2O) 2] was synthesized and its structure was determined. Cu(Ⅱ) is five coordinated in a tetragonal pyramid geometry. The two coordinating water molecules are different and the two Cu-O bond lengths differ by nearly 0.02 nm. The whole crystal is linked to form a three dimensional network by means of hydrogen bonds. The X band ESR spectrum shows three different g tensors with a well resolved hyperfine structure in the g z signal, giving the ESR parameters g x=2 05, g y =2 065 and g z =2 29. The covalency of the coordinate bonds and the deviation from tetragonal pyramid geometry for the complex are discussed based on the ESR spectra.展开更多
Hydrothermal reaction of MgCl2 and ethyl tetrazolate-5-carboxylate at 160 ℃unexpectedly yielded compound {(H3O)[Mg(H2O)6]Cl3} (1). The result of X-ray diffraction analysis indicates that 1 crystallizes in the m...Hydrothermal reaction of MgCl2 and ethyl tetrazolate-5-carboxylate at 160 ℃unexpectedly yielded compound {(H3O)[Mg(H2O)6]Cl3} (1). The result of X-ray diffraction analysis indicates that 1 crystallizes in the monoclinic system, space group C2/c with a = 9.2896(3), b = 9.5570(4), c = 13.3169(5) A, β = 90.1221(12)°, V= 1182.28(8) A3, Z = 4, Mr = 257.78, Dc = 1.448 g/cm3, μ = 0.824 mm^-1, F(000) = 536, R = 0.0265 and wR - 0.0706. 1 is composed of one hexa-aqua-magnesium(Ⅱ) ion, one hydroxonium ion, and three chlorine anions. These three components weave a perfect three-dimensional (3D) (4,4,6,12)-connected hydrogen bonding network within 1.展开更多
The title compound [In(H2ip)(pdc)(H2O)] (H3ip = 5-hydroxyisophthalic acid, H2Pdc = pyridine-2,6-dicarboxylic acid) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crysta...The title compound [In(H2ip)(pdc)(H2O)] (H3ip = 5-hydroxyisophthalic acid, H2Pdc = pyridine-2,6-dicarboxylic acid) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 13.830(8), b = 6.488(4), c = 17.632(10)A^°, β = 92.510(10)°, C15H10InNO10, Mr= 479.06, V = 1580.6(15)A^°3, Z = 4, De= 2.013 g/cm^3, F(000) = 944,μ = 1.557 mm^-1, the final R = 0.0413 and wR = 0.0793 for 2950 observed reflections with I 〉 2σ(I). The In(Ⅲ) ion is seven-coordinated in a slightly distorted penta-bipyramidal geometry. The mixed ligands connect the In(Ⅲ) ions into 21 helical chains along the [010] direction, and the hydrogen bonds assemble the chains into a three-dimensional supramolecular network.展开更多
By using a flexible multidentate ligand,bis(2-hydroxyethyl)iminotris(hydroxyhydroxylmethy)methane('bis-tris':H5L),the title complex {[Na(H6L)2]2}n·nV10O28(1) has been successfully synthesized under s...By using a flexible multidentate ligand,bis(2-hydroxyethyl)iminotris(hydroxyhydroxylmethy)methane('bis-tris':H5L),the title complex {[Na(H6L)2]2}n·nV10O28(1) has been successfully synthesized under self-assembly condition and characterized by IR spectroscopy,elemental analysis,PXRD and single-crystal X-ray diffraction.The crystal structure belongs to an orthorhombic system,space group Cmca with a = 23.752(2),b = 13.5360(8),c = 18.5377(11) ,V = 5960.1(7),Z = 8,Dc = 2.055 g/cm3,F(000) = 3744,μ = 1.630 mm-1,the final R = 0.0283 and wR = 0.0759 for 3353 observed reflections with I 〉 2σ(I).This complex consists of decavanadate [V10O28]6-motifs as counter anions intercalated with one-dimensiond chains of the composition [Na(H6L)2]n3n+.And significant intermolecular O-H…O hydrogen-bonding interactions lead to a three-dimensional supramolecular framework.展开更多
The title compound (C14H12N2O2, Mr = 240.26) crystallizes in the monoclinic system, space group P21/a with a = 7.394(1), b = 21.334(3), c = 7.423(1) ? b = 89.82(1)? V = 1170.8(3) ?, Z = 4, Dc = 1.363 g/cm3, m(MoKa) = ...The title compound (C14H12N2O2, Mr = 240.26) crystallizes in the monoclinic system, space group P21/a with a = 7.394(1), b = 21.334(3), c = 7.423(1) ? b = 89.82(1)? V = 1170.8(3) ?, Z = 4, Dc = 1.363 g/cm3, m(MoKa) = 0.93 cm-1 and F(000) = 504.00. The final R and wR are 0.0440 and 0.1370 for 2153 observed reflections (I > 2s(I)), respectively. The dihedral angle between the two phenyl rings is 52.9 and that between the NO2 group and its attached ring is 3.0. In the crystal, molecules are stacked along [100] through p…p interactions. The CH…O hydrogen bond (3.403 ? 120.4? laterally connects the stacks along [010] to form networks (001) which are further anti- parallelly connected by CH…O (3.382 ? 142.9) and p…p interactions extending along [001]. Also presented here is a brief study on the CH…O hydrogen bonds in nitro-substituted benzyl-ideneanilines which can be classified into five types, namely, )5(12R, )4(21R, )8(22R, )6(12R and )7(22R, with the first three occurring more often.展开更多
Some functional lanthanide metal complexes, such as acetylacetonato complexes, ethylenediaminetetraacetato complexes, were successfully applied for diagnostic technique. The authors are interested in investigating the...Some functional lanthanide metal complexes, such as acetylacetonato complexes, ethylenediaminetetraacetato complexes, were successfully applied for diagnostic technique. The authors are interested in investigating the structure and bonding in lanthanide and actinide metal complexes using 166Er, t55Gd, and 237Np Mtissbauer spectroscopies in connection with single-crystal and/or powder X-ray diffraction, making clear the differences on their structures as well as the differences in the participation of 4f and 5f orbitals in the chemical bonds. In this article, the crystal structures of two novel Gd(Ⅲ) acetylacetonato complexes, Gd(pta)3 · 2H2O (pta = 1,1,1 -trifluoro-5,5-dimethy 1-2,4-hexanedione) and Gd(bfa)3 · 2H2O (bfa = 1, 1, 1 -trifluoro-4-phenyl-2-4-butanedione) were reported. Though both of them were dihydrate and had distorted square antiprismatical structure, Gd(pta)3 · 2H2O crystallizes in the P 2 1/n (#14) monoclinic space group and its lattice parameters are a = 1.4141(6) nm, b = 1.0708(3) nm, c =2.2344(4) nm, β =952.4(2)°, and Gd(bfa)3· 2H2O crystallizes in P 212121 orthorhombic space group and its lattice parameters were a = 1.322 (1) nm, b = 2.295 (1) nm, c = 1. 0786(8) nm. In the meantime, the authors had finished a systematic investigation on the ^155Gd Mossbauer isomer shift (δ) of various Gd(Ⅲ) metal complexes having a different coordination number (C.N.) and different ratios coordinating oxygen to nitrogen. A tendency for the 6 value to decrease with an increase in the C.N, and the number of the nitrogen atom coordinating to Gd was confirmed. This indicated that the Gd-O and/or Gd-N bond in the investigated Gd(Ⅲ) metal complexes had a small covalent contribution, which was possible to be deduced from the O and/or N atoms of the lisands donating electrons to 6s, 5d, and 4f orbitals of Gd.展开更多
A zinc(II) complex [Zn(bdc)(py)·H 2O] n (bdc=1,4-benzenedicarboxylate, py=pyridine) has been prepared and characterized. Single crystal X-ray diffraction analysis reveals that the complex crystallizes in the mo...A zinc(II) complex [Zn(bdc)(py)·H 2O] n (bdc=1,4-benzenedicarboxylate, py=pyridine) has been prepared and characterized. Single crystal X-ray diffraction analysis reveals that the complex crystallizes in the monoclinic space group P2 1/n with a=0.84823(3), b=0.91440(3), c=1.65141(2) nm, β=91.243(2)°, V=1.28057(6) nm 3, Z=4. The coordination geometry at each Zn(II) center is a distorted tetrahedron. Two independent bdc ligands in a herringbone pattern link alternatively four-coordinated Zn(II) centers into a one-dimensional polymeric chain. Hydrogen bonds among coordinated water molecules and uncoordinated oxygen atoms of two independent bdc ligands from different polymeric chains extend one-dimensional polymeric chains into a three-dimensional structure.展开更多
The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/...The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I > 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)–C(2)=C(3)– C(4) (plane 3) and the dihedral angle between them is 14.8o. The phenone O(1) atom deviates from plane 3 by 0.291 ?. In the crystal the molecules form H-bond chains of R2 (6) and R2 (5) types 1 1 along [001]. The molecule chains interacted through three cooperative C–H…O H-bonds (R3 (11)) 1 in the ‘bay area’ (Fig. 3), extending along [010] and forming layer (100). Between the layers, there exist C–H/π interactions along [101]. Studies on the cooperative C–H…O H-bonds R3 (11) in the 1 similar crystals are also presented.展开更多
A new dinuclear centrosymmetric complex [LaL(HL)(H2O)3]2(2H2O (H2L = 3-nitrophthalic acid, NPA) was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The com...A new dinuclear centrosymmetric complex [LaL(HL)(H2O)3]2(2H2O (H2L = 3-nitrophthalic acid, NPA) was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The complex crystallizes in triclinic system, space group P1^- with a = 8.1549(16), b = 8.8856(18), c = 15.277(3)A,α= 100.93(3),α= 90.81(3), γ= 104.56(3)°, V = 1049.8(4)A^3, Z = 1,μ= 2.125 mm^-1, Dc=1.994 g/cm^3, R = 0.0259 and wR = 0.0679. Two 3-nitrophthalates(2-) coordinate with the La3+ ions in a bridging mode, and two monohydrogen- 3-nitrophthates(1-) and three waters in terminal ways, respectively. Each La^3+ ion is nine-coordinated to exhibit a distorted tricapped trigonal prism coordination polyhedron. Both the coordinated and crystal waters are involved in the inter- and intramolecular hydrogen bonds. The dinuclear units are linked into a 2D network structure in the ab plane via intermolecular hydrogen bonds along the axes a and b. Two crystal waters fill each rhombic pore of the network. The networks are further packed along the c axis forming a layered supramolecular structure through the C-H…O weak forces between the adjacent sheets. TGA analysis shows the complex undergoes the loss of waters of crystallization and coordination and the decomposition of ligands sequentially.展开更多
Two novel polymeric complexes, [Gd(HsTCAS)(H2O)7]·4H2O 1 and [Gd(HsTCAS) (CH3COCH3)(H2O)6]·6H2O 2 (H4TCAS = p-sulfonatothiacalix[4]arene), have been synthesized and characterized by single-crysta...Two novel polymeric complexes, [Gd(HsTCAS)(H2O)7]·4H2O 1 and [Gd(HsTCAS) (CH3COCH3)(H2O)6]·6H2O 2 (H4TCAS = p-sulfonatothiacalix[4]arene), have been synthesized and characterized by single-crystal X-ray diffraction analyses. Complex 1 crystallizes in monoclinic, space group C2/m with a = 20.2308(12), b = 19.0894(10), c = 12.2448(7)A, β = 101.847(3)°, V = 4628.1(5)A^3, C24H43GdO27S8, Mr = 1169.25, Z = 4, Dc = 1.690 g/cm^3, F(000) = 2380,μ = 1.879 mm^-1, the final R = 0.0404 and wR = 0.1038 for 5127 observed reflections with I 〉 2σ(I). Complex 2 is pseudo-isostructural with complex 1.展开更多
A hydrogen-bonded three-dimensional cobalt(II) compound, {[Co(2,2?-bipy)- (Hbtc)(H2O)3]3H2O}n 1 (H3btc = 1,3,5-benzenetricarboxylic acid, 2,2?-bipy = 2,2?-bipyridine), has been synthesized and characterized by single-...A hydrogen-bonded three-dimensional cobalt(II) compound, {[Co(2,2?-bipy)- (Hbtc)(H2O)3]3H2O}n 1 (H3btc = 1,3,5-benzenetricarboxylic acid, 2,2?-bipy = 2,2?-bipyridine), has been synthesized and characterized by single-crystal X-ray diffraction analysis, IR and TGA. Compound 1 crystallizes in monoclinic, space groups P21/n, C19H36CoN2O12, Mr = 543.43, a = 7.6930(2), b = 19.3715(6), c = 15.9408(5) , = 95.8750(10)o, V = 2363.10(12) 3, Z = 4, Dc = 1.527 g/cm3, = 0.792 mm1, F(000) = 1148, R = 0.0489 and wR = 0.1437 for 4085 reflections. The Co(II) atom is coordinated by an oxygen atom of monodentate Hbtc2, two nitrogen atoms of 2,2?-bipy and three water molecules into a slightly distorted octahedral geometry. The inter- molecular hydrogen bonding interactions among the adjacent [Co(2,2?-bipy)(Hbtc)(H2O)3] extend the compound into a three-dimensional porous supramolecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.展开更多
The crystal of aconitine has been obtained through an unexpected spontaneous change of the solid power of aconitine in air and characterized by single-crystal X-ray diffraction analysis and elemental analysis. Crystal...The crystal of aconitine has been obtained through an unexpected spontaneous change of the solid power of aconitine in air and characterized by single-crystal X-ray diffraction analysis and elemental analysis. Crystallographic data: orthorhombic, space group P2_12_12_1 with a = 17.0745(6), b = 15.5990(6), c = 12.2443(6) ?, V = 3261.2(2) ?~3, Z = 4, C_(34)H_(47)NO_(11), M_r = 645.73, D_c = 1.315 g/cm^3, F(000) = 1384, μ(MoKa) = 0.098 mm^(-1), R = 0.0605 and wR = 0.1311. Aconitine is diester diterpenoid alkaloid, and its main structure is composed of four six-membered and two five-membered rings. The intramolecular and intermolecular O–H···O and C–H···O hydrogen bonds extend the adjacent molecules into a one-dimensional chain and a two-dimensional framework, which may be the essential reason for the change.展开更多
The title compounds, Cu(L1)(C4H8NHO) and Ni(L2)(C4H8NHO) (H2L1 = 5-bromosalicylaldehyde-p-nitrobenzoylhydrazone, H2L2 = 5-bromosalicylaldehyde-p-hydroxybenzoylhydrazone), have been obtained and characterized...The title compounds, Cu(L1)(C4H8NHO) and Ni(L2)(C4H8NHO) (H2L1 = 5-bromosalicylaldehyde-p-nitrobenzoylhydrazone, H2L2 = 5-bromosalicylaldehyde-p-hydroxybenzoylhydrazone), have been obtained and characterized by single-crystal X-ray diffraction. Complex 1 belongs to the triclinic system, space group P1 with a = 8.6960(2), b = 9.957(2), c = 11.878(2)A, α = 73.36(3), β = 78.25(3), γ = 82.64(3)°, V = 962.1(3) A^3, Mr= 512.81, Z = 2, F(000) = 514, Dc = 1.770 g/cm^3,μ(MoKα) = 3.251, R = 0.0337 and wR = 0.0846. Complex 2 is of monoclinic, space group P21/c with a = 13.313(2), b = 8.2096(1), c = 21.890(3) A,β = 125.737(3)°, V = 1941.9(4) A^3, Mr= 478.97, Z = 4, F(000) = 968, Dc = 1.638 g/cm^3,μ(MoKα) = 3.085, R = 0.0356 and wR = 0.0817. The ligands form a satisfactory N2O2 square plane around the metal centers in two compounds. Different patterns of hydrogen bonds are observed owing to the presence of different substituents on aromatic ring of the acylhydrazone Schiff bases. In complex 1, square-planar copper(Ⅱ) complexes are linked by intermolecular hydrogen bonds leading to zigzag infinite chains. In complex 2, the metal complexes are linked via hydrogen bonds to form corrugated sheets in a staggered fashion; 3D channels along the b axis are constructed through other non-covalent interactions between the neighboring layers.展开更多
基金supported by the National Natural Science Foundation of China (No. 29890210) and the Key Project of the Chinese Academy of Sciences (KJCX2-H3)
文摘The assembly of 1,4-benzenedicarboxylic acid (H2bdc), 4,4?bipyridine (4,4?bipy), trimethyltin chloride and MnBr24H2O in hydrothermal conditions gave rise to a hydrogen-bonded three-dimensional complex {[Mn(4,4?bipy)4H2O](bdc)}n which has been characterized by single- crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group P2/n with a = 7.0001(2), b = 11.5540(3), c = 11.4192(1) ? = 101.754(2)? V = 904.21(4) 3, Z = 2, C18H20MnN2O8, Mr = 447.30, Dc = 1.643 g/cm3, F(000) = 462 and m(MoK? = 0.783 mm-1. The final R and wR are 0.0499 and 0.1301, respectively for 1335 observed reflections with I ≥ 2(I). The Mn (Ⅱ) is six-coordinated in a distorted octahedral geometry. 4,4?Bipyridine in a m-bridge mode links [Mn(H2O)4]2+ into a linear cation chain. bdc acts as a counter anion and links the linear chains into a three-dimensional structure through hydrogen bonds.
基金This work was supported by the National Natural Science Foundation of China and Natural Science Foundation of Fujian Province
文摘A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·2C3H7OH·2H2O 1 (abo = R(-)-2-amino-1-butanol) has been synthesized from VO2^+ in organic solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a = 11.419(9), b = 16.811(16), c = 15.521(12) A, β= 102.98(2)°, V= 2903(4) A^3, Z = 4, C15H46N3O19V5, Mr = 827.25, Dc = 1.893 g/cm^3, 2(MoKα) = 0.71073 A, μ = 1.636 mm^-1, F(000) = 1696, the final R = 0.0696 and wR = 0.1361 for 4641 observed reflections with I 〉 2σ(I). The compound is based on decavanadate clusters [V10O28]^6-. The hydrogen bonding interactions among Habo^+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.
基金This work was supported by the National Natural Science Foundation of China (Nos. 20671011, 20331010, 90406002 and 90406024)the 111 Project (B07012) and Key Laboratory of Structural Chemistry Foundation (No. 060017)
文摘A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu(naphdien)]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490(15), b = 7.0847(16), c = 30.845(3)A, β= 95.33(3)°, V = 1599.0(5)A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F(000) = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones (I 〉2σ(I)). In the crystal structure, mononuclear units [Cu(naphdien)]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.
基金This work was supported by the National Natural Science Foundation of China (No. 20231020)
文摘Two zinc(Ⅱ) compounds, [Zn(L)(H2O)2]n 1 and [Zn(4,4'-bpy)(H2O)4](L) 2 (H2L = trans,trans-1,3 butadiene 1,4-dicarboxylic acid), were synthesized by hydrothermal methods and characterized by single-crystal X-ray diffraction analyses. Compound 1 crystallizes in monoclinic, space group C2/c with a=15.4970(16), b = 5.4976(6), c = 10.7113(12) A, β=96.298(6)°, C6H8O6Zn, Mr = 241.50, V = 907.06(17) A^3, Z = 4, D, = 1.768 g/cm^3, F(000) = 488,μ = 2.703 mm^-1, S = 1.060, the final R = 0.0256 and wR = 0.0660 for 968 observed reflections with Ⅰ 〉 2σ(Ⅰ). Compound 2 crystallizes in triclinic, space group P1^- with a = 6.915(2), b = 7.166(2), c = 10.363(3) A, α = 73.250(4), β = 84.429(4), γ = 61.605(3)°, C16H2ON2O8Zn, Mr = 433.70, V = 432.1 (2) A^3, Z = 1, D, = 1.667 g/cm^3, F(000) = 224 and μ= 1.471 mm^-1, S = 1.118, the final R = 0.0486 and wR = 0.1077 for 1352 observed reflections with Ⅰ〉 2σ(Ⅰ). Upon using the assembly strategy of combination of coordination polymer chains with intermolecular hydrogen bonds, three-dimensional frameworks of complexes 1 and 2 were formed.
基金This work was supported by the Outstanding Young Foundation of Henan Province
文摘The supramolecular compound [(AgI3)(4-HBPFA)2(H2O)] (Mr = 1361.11) was synthesized via the reaction of 1,1?-bis[(4-pyridylamino)carbonyl]ferrocene (4-BPFA) with AgI, and structurally characterized by single-crystal X-ray diffraction analysis. Crystal data: monoclinic, space group C2/c, a = 1.6783(3), b = 10.646(2), c = 2.5419(5) ?, β = 93.66(3)o, V = 4532.2(16) ?3, Z = 4, Dc = 1.995 g/cm3, F(000) = 2632 and μ = 3.158 mm-1. The compound consists of (4- HBPFA)+, (AgI3)2- and H2O. In the structure, the adjacent (4-HBPFA)+ are linked by C–H…O and N–H…N hydrogen bonds into 1-D chains which are further linked by C–H…I and N–H…I hydrogen bonds as well as intermolecular π-π stacking interactions to form a 3-D supramolecular compound.
基金This work was supported by the National Natural Science Foundation of China (90206040 20325106) Natural Science Foundation of Fujian Province (B982003) and the Key and "One Hundred Talent" Projects from CAS.
文摘The title compound, {[Cu(2,2?-bipy)(C7H4O5S)(H2O)2]?H2O}n (2,2?-bipy = 2,2?- bipyridine), was synthesized by the hydrothermal reaction of Cu(NO3)2?3H2O, 2,2?-bipyridine and 2-sulphobenzoic acid, and structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of triclinic, space group P1 with a = 9.21(3), b = 10.17(3), c = 10.77(3) ?, α = 77.017(16), β = 89.80(8), γ = 68.46(7)°, V = 911(5) ?3, Z = 2, (D/s)max= 0.001, Mr = 473.94, Dc = 1.728 g/cm3, μ(MoKα) = 1.365 mm-1, F(000) = 486, the final R = 0.0246 and wR = 0.0628 for 3809 observed reflections with I > 2σ(I). The mononuclear crystal structure extends into a two-dimensional net- work via hydrogen-bonding interactions and a three-dimensional framework is further formed by means of π-π stacking interactions.
基金supported by the Postdoctor Foundation of Jiangsu Province (No. 0701001B)the Foundation of Taishan University (No. Y04-2-02)
文摘A manganese(Ⅱ) complex (tataH)2[Mn(pydc)2]·4H2O (C20H28MBN14O12, Mr = 711.50, tata = 2,4,6-triamino-1,3,5-triazine, pydcH2 = pyridine-2,6-dicarboxylic acid) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1^-, with a = 9.9847(3), b = 10.9813(3), c = 15.2616(5)A, a = 101.5310(10), β = 90.2610(10), γ = 116.4600( 10)% V = 1459.44(8)A^3, Z = 2, Dc = 1.619 g/cm^3,μ = 0.539 mm^-1, F(000) = 734, the final R = 0.0292 and wR = 0.0745. In the crystal the Mnn atom is six-coordinated by four carbonyl oxygen atoms and two pyridine nitrogen atoms from two tridentate pydc ligands to furnish a distorted octahedral geometry. The complex shows the A…D…D'…A' H-bonded tetramer. The molecules are packed in a three-dimensional framework structure by the combination of O-H…O, N-H…O and N-H…N hydrogen bonds between (tataH)^+, [Mn(pydc)2]^2- and crystal water.
基金Supported by the National Natural Science Foundation of China(No.2 0 0 710 192 0 0 710 2 0 and5 0 172 0 2 ) and the Re-search Fund for Doctoral Program of Higher Education.
文摘A new copper(Ⅱ) complex [Cu(PDA)(H 2O) 2] was synthesized and its structure was determined. Cu(Ⅱ) is five coordinated in a tetragonal pyramid geometry. The two coordinating water molecules are different and the two Cu-O bond lengths differ by nearly 0.02 nm. The whole crystal is linked to form a three dimensional network by means of hydrogen bonds. The X band ESR spectrum shows three different g tensors with a well resolved hyperfine structure in the g z signal, giving the ESR parameters g x=2 05, g y =2 065 and g z =2 29. The covalency of the coordinate bonds and the deviation from tetragonal pyramid geometry for the complex are discussed based on the ESR spectra.
基金Supported by the Youth Foundation of Jiangxi Provincial Office of Education (GJJ09605)the Science Foundation of Jiangxi Provincial Office of Education (GJJ09637)
文摘Hydrothermal reaction of MgCl2 and ethyl tetrazolate-5-carboxylate at 160 ℃unexpectedly yielded compound {(H3O)[Mg(H2O)6]Cl3} (1). The result of X-ray diffraction analysis indicates that 1 crystallizes in the monoclinic system, space group C2/c with a = 9.2896(3), b = 9.5570(4), c = 13.3169(5) A, β = 90.1221(12)°, V= 1182.28(8) A3, Z = 4, Mr = 257.78, Dc = 1.448 g/cm3, μ = 0.824 mm^-1, F(000) = 536, R = 0.0265 and wR - 0.0706. 1 is composed of one hexa-aqua-magnesium(Ⅱ) ion, one hydroxonium ion, and three chlorine anions. These three components weave a perfect three-dimensional (3D) (4,4,6,12)-connected hydrogen bonding network within 1.
基金supported by 973 Program (2006CB932900)NNSFC (20571074)NSF of Fujian Province (2007J172)
文摘The title compound [In(H2ip)(pdc)(H2O)] (H3ip = 5-hydroxyisophthalic acid, H2Pdc = pyridine-2,6-dicarboxylic acid) has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 13.830(8), b = 6.488(4), c = 17.632(10)A^°, β = 92.510(10)°, C15H10InNO10, Mr= 479.06, V = 1580.6(15)A^°3, Z = 4, De= 2.013 g/cm^3, F(000) = 944,μ = 1.557 mm^-1, the final R = 0.0413 and wR = 0.0793 for 2950 observed reflections with I 〉 2σ(I). The In(Ⅲ) ion is seven-coordinated in a slightly distorted penta-bipyramidal geometry. The mixed ligands connect the In(Ⅲ) ions into 21 helical chains along the [010] direction, and the hydrogen bonds assemble the chains into a three-dimensional supramolecular network.
基金supported by 973 Program (2011CB932504), NNSFC (20971121)NSF for Young Scientists of China (20801056)NSF of Fujian Province
文摘By using a flexible multidentate ligand,bis(2-hydroxyethyl)iminotris(hydroxyhydroxylmethy)methane('bis-tris':H5L),the title complex {[Na(H6L)2]2}n·nV10O28(1) has been successfully synthesized under self-assembly condition and characterized by IR spectroscopy,elemental analysis,PXRD and single-crystal X-ray diffraction.The crystal structure belongs to an orthorhombic system,space group Cmca with a = 23.752(2),b = 13.5360(8),c = 18.5377(11) ,V = 5960.1(7),Z = 8,Dc = 2.055 g/cm3,F(000) = 3744,μ = 1.630 mm-1,the final R = 0.0283 and wR = 0.0759 for 3353 observed reflections with I 〉 2σ(I).This complex consists of decavanadate [V10O28]6-motifs as counter anions intercalated with one-dimensiond chains of the composition [Na(H6L)2]n3n+.And significant intermolecular O-H…O hydrogen-bonding interactions lead to a three-dimensional supramolecular framework.
文摘The title compound (C14H12N2O2, Mr = 240.26) crystallizes in the monoclinic system, space group P21/a with a = 7.394(1), b = 21.334(3), c = 7.423(1) ? b = 89.82(1)? V = 1170.8(3) ?, Z = 4, Dc = 1.363 g/cm3, m(MoKa) = 0.93 cm-1 and F(000) = 504.00. The final R and wR are 0.0440 and 0.1370 for 2153 observed reflections (I > 2s(I)), respectively. The dihedral angle between the two phenyl rings is 52.9 and that between the NO2 group and its attached ring is 3.0. In the crystal, molecules are stacked along [100] through p…p interactions. The CH…O hydrogen bond (3.403 ? 120.4? laterally connects the stacks along [010] to form networks (001) which are further anti- parallelly connected by CH…O (3.382 ? 142.9) and p…p interactions extending along [001]. Also presented here is a brief study on the CH…O hydrogen bonds in nitro-substituted benzyl-ideneanilines which can be classified into five types, namely, )5(12R, )4(21R, )8(22R, )6(12R and )7(22R, with the first three occurring more often.
基金Project supported by the Grants-in-Aid for Scientific Research from the Ministry of Education, Science and Culture, Japan andin Part by the Inter-University Joint Research Program for the Common Use of JAERI (Japan Atomic Energy Research Institute)Facilities
文摘Some functional lanthanide metal complexes, such as acetylacetonato complexes, ethylenediaminetetraacetato complexes, were successfully applied for diagnostic technique. The authors are interested in investigating the structure and bonding in lanthanide and actinide metal complexes using 166Er, t55Gd, and 237Np Mtissbauer spectroscopies in connection with single-crystal and/or powder X-ray diffraction, making clear the differences on their structures as well as the differences in the participation of 4f and 5f orbitals in the chemical bonds. In this article, the crystal structures of two novel Gd(Ⅲ) acetylacetonato complexes, Gd(pta)3 · 2H2O (pta = 1,1,1 -trifluoro-5,5-dimethy 1-2,4-hexanedione) and Gd(bfa)3 · 2H2O (bfa = 1, 1, 1 -trifluoro-4-phenyl-2-4-butanedione) were reported. Though both of them were dihydrate and had distorted square antiprismatical structure, Gd(pta)3 · 2H2O crystallizes in the P 2 1/n (#14) monoclinic space group and its lattice parameters are a = 1.4141(6) nm, b = 1.0708(3) nm, c =2.2344(4) nm, β =952.4(2)°, and Gd(bfa)3· 2H2O crystallizes in P 212121 orthorhombic space group and its lattice parameters were a = 1.322 (1) nm, b = 2.295 (1) nm, c = 1. 0786(8) nm. In the meantime, the authors had finished a systematic investigation on the ^155Gd Mossbauer isomer shift (δ) of various Gd(Ⅲ) metal complexes having a different coordination number (C.N.) and different ratios coordinating oxygen to nitrogen. A tendency for the 6 value to decrease with an increase in the C.N, and the number of the nitrogen atom coordinating to Gd was confirmed. This indicated that the Gd-O and/or Gd-N bond in the investigated Gd(Ⅲ) metal complexes had a small covalent contribution, which was possible to be deduced from the O and/or N atoms of the lisands donating electrons to 6s, 5d, and 4f orbitals of Gd.
基金ProjectsupportedbytheNationalNaturalScienceFoundationofChina (No .2 982 5 10 3) ,theNaturalScienceFoundation (No .8982 0 0 3)ofFujianProvinceandChineseAcademyofSciences
文摘A zinc(II) complex [Zn(bdc)(py)·H 2O] n (bdc=1,4-benzenedicarboxylate, py=pyridine) has been prepared and characterized. Single crystal X-ray diffraction analysis reveals that the complex crystallizes in the monoclinic space group P2 1/n with a=0.84823(3), b=0.91440(3), c=1.65141(2) nm, β=91.243(2)°, V=1.28057(6) nm 3, Z=4. The coordination geometry at each Zn(II) center is a distorted tetrahedron. Two independent bdc ligands in a herringbone pattern link alternatively four-coordinated Zn(II) centers into a one-dimensional polymeric chain. Hydrogen bonds among coordinated water molecules and uncoordinated oxygen atoms of two independent bdc ligands from different polymeric chains extend one-dimensional polymeric chains into a three-dimensional structure.
基金This research was supported by the Key Subject Foundation of Jiangsu Province(S1109001)
文摘The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I > 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)–C(2)=C(3)– C(4) (plane 3) and the dihedral angle between them is 14.8o. The phenone O(1) atom deviates from plane 3 by 0.291 ?. In the crystal the molecules form H-bond chains of R2 (6) and R2 (5) types 1 1 along [001]. The molecule chains interacted through three cooperative C–H…O H-bonds (R3 (11)) 1 in the ‘bay area’ (Fig. 3), extending along [010] and forming layer (100). Between the layers, there exist C–H/π interactions along [101]. Studies on the cooperative C–H…O H-bonds R3 (11) in the 1 similar crystals are also presented.
基金This work was supported by the Beijing Talent Fund for Young Sci-Tech Researchers (No. H013610050112)
文摘A new dinuclear centrosymmetric complex [LaL(HL)(H2O)3]2(2H2O (H2L = 3-nitrophthalic acid, NPA) was synthesized in water/ethanol solution and characterized by X-ray diffraction, IR spectrum and TGA-DTA. The complex crystallizes in triclinic system, space group P1^- with a = 8.1549(16), b = 8.8856(18), c = 15.277(3)A,α= 100.93(3),α= 90.81(3), γ= 104.56(3)°, V = 1049.8(4)A^3, Z = 1,μ= 2.125 mm^-1, Dc=1.994 g/cm^3, R = 0.0259 and wR = 0.0679. Two 3-nitrophthalates(2-) coordinate with the La3+ ions in a bridging mode, and two monohydrogen- 3-nitrophthates(1-) and three waters in terminal ways, respectively. Each La^3+ ion is nine-coordinated to exhibit a distorted tricapped trigonal prism coordination polyhedron. Both the coordinated and crystal waters are involved in the inter- and intramolecular hydrogen bonds. The dinuclear units are linked into a 2D network structure in the ab plane via intermolecular hydrogen bonds along the axes a and b. Two crystal waters fill each rhombic pore of the network. The networks are further packed along the c axis forming a layered supramolecular structure through the C-H…O weak forces between the adjacent sheets. TGA analysis shows the complex undergoes the loss of waters of crystallization and coordination and the decomposition of ligands sequentially.
基金This work was supported by the National Natural Science Foundation of China,Natural Science Foundation of Fujian Province,and the Young Scientist Funds of Fujian Province (No. 2006F3130)
文摘Two novel polymeric complexes, [Gd(HsTCAS)(H2O)7]·4H2O 1 and [Gd(HsTCAS) (CH3COCH3)(H2O)6]·6H2O 2 (H4TCAS = p-sulfonatothiacalix[4]arene), have been synthesized and characterized by single-crystal X-ray diffraction analyses. Complex 1 crystallizes in monoclinic, space group C2/m with a = 20.2308(12), b = 19.0894(10), c = 12.2448(7)A, β = 101.847(3)°, V = 4628.1(5)A^3, C24H43GdO27S8, Mr = 1169.25, Z = 4, Dc = 1.690 g/cm^3, F(000) = 2380,μ = 1.879 mm^-1, the final R = 0.0404 and wR = 0.1038 for 5127 observed reflections with I 〉 2σ(I). Complex 2 is pseudo-isostructural with complex 1.
基金This work was supported by the National Natural Science Foundation of China Natural Science Foundation of Fujian Province and the Key Project of the Chinese Academy of Sciences
文摘A hydrogen-bonded three-dimensional cobalt(II) compound, {[Co(2,2?-bipy)- (Hbtc)(H2O)3]3H2O}n 1 (H3btc = 1,3,5-benzenetricarboxylic acid, 2,2?-bipy = 2,2?-bipyridine), has been synthesized and characterized by single-crystal X-ray diffraction analysis, IR and TGA. Compound 1 crystallizes in monoclinic, space groups P21/n, C19H36CoN2O12, Mr = 543.43, a = 7.6930(2), b = 19.3715(6), c = 15.9408(5) , = 95.8750(10)o, V = 2363.10(12) 3, Z = 4, Dc = 1.527 g/cm3, = 0.792 mm1, F(000) = 1148, R = 0.0489 and wR = 0.1437 for 4085 reflections. The Co(II) atom is coordinated by an oxygen atom of monodentate Hbtc2, two nitrogen atoms of 2,2?-bipy and three water molecules into a slightly distorted octahedral geometry. The inter- molecular hydrogen bonding interactions among the adjacent [Co(2,2?-bipy)(Hbtc)(H2O)3] extend the compound into a three-dimensional porous supramolecular framework. The uncoordinated water molecules act as space-fillers and consolidate the whole architecture through the hydrogen bonding interactions.
基金Supported by the Scientific Research Project of Education Department of Shaanxi Provincial Government in 2014(No.14JK1045)the key project of Baoji University of Arts and Sciences in 2014(No.ZK14009)
文摘The crystal of aconitine has been obtained through an unexpected spontaneous change of the solid power of aconitine in air and characterized by single-crystal X-ray diffraction analysis and elemental analysis. Crystallographic data: orthorhombic, space group P2_12_12_1 with a = 17.0745(6), b = 15.5990(6), c = 12.2443(6) ?, V = 3261.2(2) ?~3, Z = 4, C_(34)H_(47)NO_(11), M_r = 645.73, D_c = 1.315 g/cm^3, F(000) = 1384, μ(MoKa) = 0.098 mm^(-1), R = 0.0605 and wR = 0.1311. Aconitine is diester diterpenoid alkaloid, and its main structure is composed of four six-membered and two five-membered rings. The intramolecular and intermolecular O–H···O and C–H···O hydrogen bonds extend the adjacent molecules into a one-dimensional chain and a two-dimensional framework, which may be the essential reason for the change.
基金Special Foundation for Young Scientists of Fuzhou University (XRC-0644)Sci.& Tech.Promotion Foundation of Fuzhou University (XJJ-0605)
文摘The title compounds, Cu(L1)(C4H8NHO) and Ni(L2)(C4H8NHO) (H2L1 = 5-bromosalicylaldehyde-p-nitrobenzoylhydrazone, H2L2 = 5-bromosalicylaldehyde-p-hydroxybenzoylhydrazone), have been obtained and characterized by single-crystal X-ray diffraction. Complex 1 belongs to the triclinic system, space group P1 with a = 8.6960(2), b = 9.957(2), c = 11.878(2)A, α = 73.36(3), β = 78.25(3), γ = 82.64(3)°, V = 962.1(3) A^3, Mr= 512.81, Z = 2, F(000) = 514, Dc = 1.770 g/cm^3,μ(MoKα) = 3.251, R = 0.0337 and wR = 0.0846. Complex 2 is of monoclinic, space group P21/c with a = 13.313(2), b = 8.2096(1), c = 21.890(3) A,β = 125.737(3)°, V = 1941.9(4) A^3, Mr= 478.97, Z = 4, F(000) = 968, Dc = 1.638 g/cm^3,μ(MoKα) = 3.085, R = 0.0356 and wR = 0.0817. The ligands form a satisfactory N2O2 square plane around the metal centers in two compounds. Different patterns of hydrogen bonds are observed owing to the presence of different substituents on aromatic ring of the acylhydrazone Schiff bases. In complex 1, square-planar copper(Ⅱ) complexes are linked by intermolecular hydrogen bonds leading to zigzag infinite chains. In complex 2, the metal complexes are linked via hydrogen bonds to form corrugated sheets in a staggered fashion; 3D channels along the b axis are constructed through other non-covalent interactions between the neighboring layers.