Synthesis and THF Accompanied Crystal Structure of 11H-Naphtho[1',2':5,6]- pyrano[2,3-d]pyrimidin-11(10H)-one

8,9,12-Trihydro-9,9-pentamethylene-12-(3-nitrophenyl)-11H-naphtho[1',25,6]-pyrano[2,3-d]pyrimidin-11(10H)-one 1,another conversion product of Friedlndler reaction,has been synthesized by the reaction of 2-amino-4-(3-nitrophenyl)-4H-benzo[f]chromene-3-carbo-nitrile 2 with cyclohexanone in the presence of Lewis acid catalysts.The crystal of the title compound 1 THF solvate,C60H62N6O10,was obtained and determined by X-ray diffraction me-thod.The crystal is of triclinic,space group P with a = 11.4633(11),b = 12.6247(12),c = 19.658(2) ,α = 72.642(8),β = 89.045(9),γ = 68.340(5)°,V = 2509.6(4),Z = 2,Dc = 1.359 g/cm3,F(000) = 1088,Mr = 1027.16,the final R = 0.0674 and wR = 0.1869 with Ⅰ > 2σ(Ⅰ) and the goodness-of-fit S = 1.045 on F2.The pyrimidine ring has an envelope conformation,linked with a six-membered ring through a spiro C atom.The crystal packing of 1 THF solvate is stabilized by N-H···O hydrogen bonds,and π-π stacking interaction occurs between two adjacent nearly planar molecules of 1.     

Synthesis and THF Accompanied Crystal Structure of llH-Naphtho[1＇,2＇：5,6]- pyrano[2,3-d]pyrimidin- 11 （10H）-one

8,9,12-Trihydro-9,9-pentamethylene- 12-（3-nitrophenyl）- 11H-naphtho[ 1＇,25,6]- pyrano[2,3-d]pyfimidin- 11 （10H）-one 1, another conversion product of Ffiedlandler reaction, has been synthesized by the reaction of 2-amino-4-（3-nitrophenyl）-4H-benzo[f]chromene-3-carbonitrile 2 with cyclohexanone in the presence of Lewis acid catalysts. The crystal of the title compound 1 THF solvate, C60H62N6O10, was obtained and determined by X-ray diffraction method. The crystal is of triclinic, space group P1 with a = 11.4633（11）, b = 12.6247（12）, c = 19.658（2）A, α = 72.642（8）, β = 89.045（9）, γ = 68.340（5）°, V = 2509.6（4）, Z = 2, De = 1.359 g/cm^3, F（000） = 1088, Mr = 1027.16, the final R = 0.0674 and wR = 0.1869 with Ⅰ 〉 2σ（Ⅰ） and the goodness-of-fit S = 1.045 on F^2. The pyrimidine ring has an envelope conformation, linked with a six-membered ring through a spiro C atom. The crystal packing of 1 THF solvate is stabilized by N-H…O hydrogen bonds, and π-π stacking interaction occurs between two adjacent nearly planar molecules of 1.     

Synthesis and Crystal Structure of 5-Cyclopropyl- 10-（4-fluorophenyl）-7,7-dimethyl-7,8-dihydro-5H- indeno[1,2-b]quinoline-9,11（6H,10H）-dione

The title compound 5-cyclopropyl-10-(4-fluorophenyl)-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11(6H,10H)-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-(cyclopropylamino)-5,5-dimethylcyclohex-2-enone in the presence of acetic acid under microwave irradiation. Its structure was confirmed by IR and 1H- NMR spectra. The crystal is of monoclinic, space group P21/c with a = 14.138(3), b = 8.952(2), c = 17.140(3) , β = 102.253(3)o, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9(8) 3, Dc = 1.296 g/cm3, μ(MoKα) = 0.087 mm-1, F(000) = 872, the final R = 0.0425 and wR = 0.0905 for 2336 observed reflections (I > 2σ(I)). X-ray analysis revealed that the pyridine ring adopts a boat conformation and the six-membered ring fused with it assumes a twist boat conformation.     

Hydrothermal Synthesis, Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH2]2+·[SbCl5]2-}2

A new supramolecular compound, {[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetric analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 16.0397(13), b = 14.3189(12), c = 15.6370(13) (A), β = 105.8980(10)°, V = 3454.0(5) (A)3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3, μ = 2.366 mm-1, S = 1.010, F(000) = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb…C1.Moreover,the compund adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridy1)benzimidazole divalent cations.The title compound also shows godd fluorescent behaviors.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]~(2 )·[SbCl_5]~(2-)}_2

A new supramolecular compound,{[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2,was synthesized by the hydrothermal reaction of o-diaminobenzene,2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution,and characterized by chemical analysis,elemental analysis,IR spectra,thermogravimetric analysis and fluorescence spectra. The crystal structure was deter-mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system,space group P21/c,with a=16.0397(13),b=14.3189(12),c=15.6370(13),β=105.8980(10)°,V=3454.0(5)3,Z=4,C24H22Cl10N6Sb2,Mr=992.48,Dc=1.909 g/cm3,μ=2.366 mm-1,S=1.010,F(000)=1920,R=0.0254 and wR=0.0555. The coordination anion,[SbCl5]2-which is a distorted tetragonal pyramid,is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2-form a biquaternion ring structure through the secondary bonding of Sb···Cl. Moreover,the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridyl)benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [C8H8NdCl（THF）2]2

<正> The title complex was prepared from the reaction of NdClLi0.3 and C8H8, its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/c with cell dimensions o = 11. 819(3), 6=12.651(3), c=13. 478(3)A, β=122.99(2)°, Mr = 856. 00, Z = 2, Dc=1. 68g/cm3, F(000) = 636. 89, V = 1690. 33A3. The structure was solved by direct methods and Fourier techniques. Least squares refinement on the basis of 1842 observed reflections led to final R = 0. 038 and Rw = 0. 040. The molecule is a dimer of C3H8NdCl(THF)2 bridged by two Cl atoms with Nd -Cl bond lengths of 2. 832(2) A and 2. 917(3)A.     

Synthesis and Crystal Structure of 9-（2-Hydroxy-5-nitrophenyl）-9H-dibenzo[c,h]-2,7,10-trioxanthene-1,8-dione DMF Solvate

The title compound 9-(2-hydroxy-5-nitrophenyl)-9H-dibenzo[c,h]-2,7,10-trioxan-thene-1,8-dione DMF solvate (C28H20N2O9,Mr=528.46) was synthesized and crystallized.The crystal belongs to the triclinic system,space group P1 with a=10.210(3),b=10.698(4),c=12.522(4),α=92.214(6),β=113.751(5),γ=105.040(5)°,Z=2,V=1193.0(7)3,Dc=1.471 g·cm-3,μ(MoKα)=0.112 mm-1,F(000)=548,R=0.0444 and wR=0.1141 for 2667 observed reflections (I 2σ(I)).X-ray analysis reveals that atoms C(1),C(2),C(3),C(4),C(5) and O(1) on the new 4H-pyran ring are slightly distorted,forming a half-chair conformation.     

Synthesis,Crystal Structure and Antiproliferative Activity of 2-（（（5-（（（5,7-Dimethyl-[1,2,4]triazolo-[1,5-a]pyrimidin-2-yl）thio）methyl）-4-phenyl-4H-1,2,4-triazol-3-yl）thio）methyl）-4Hchromen-4-one Methanol Solvate

The novel crystal of the title compound 2-(((5-(((5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl)thio)methyl)-4-phenyl-4H-1,2,4-triazol-3-yl)thio)methyl)-4H-chromen-4-one methanol solvate(C27H25N7O3S2, Mr = 559.66) has been prepared and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monocline system, space group P21/c with a = 11.9879(9), b = 14.0743(10), c = 15.9706(11), β = 98.509(2)°, V = 2664.9(3)3, Z = 4, Dc = 1.395 g/cm3, F(000) = 1168, μ = 0.116 mm-1, MoKa radiation(λ = 0.71073), R = 0.0652, and wR = 0.1425 for 5220 observed reflections with I 2σ(I). X-ray diffraction analyses reveal that the molecule adopts a C-shape. The planes of the benzopyrone and triazolopyrimidine were nearly parallel to each other, with a dihedral angle of 1.21(3)°. Intramolecular and intermolecular hydrogen bonds together with π-π interations are found to exist in the structure. The results of MTT assay indicate that the title compound displays excellent antiproliferative activity against two human cancer cell lines.     

Synthesis and Crystal Structure of 2-Methoxy-benzoic Acid 2-Oxo-3-（2,4,6-trimethyl-phenyl）-1-oxa-spiro[4.4]non-3-en-4-yl Ester

The new title compound 2-methoxy-benzoic acid 2-oxo-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-4-yl ester(3,C25H26O5) has been synthesized by the condensation reaction of 4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-2-one(2) with 2-methoxylben-zoyl chloride,and characterized by 1H NMR and MS spectra.Its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with a = 10.6945(7),b = 12.8176(7),c = 16.4223(10) ,β = 103.5665(17)o,V = 2188.3(2) 3,Z = 4,Dc = 1.234 g/cm3,F(000) = 864.000,μ = 0.085 mm-1,the final R = 0.0520 and wR = 0.1132 for 2732 observed reflections with I 2σ(I).In the crystal structure,the C(1)-C(2)(1.478 ) bond is significantly shorter than the normal single C-C bond(1.53 ),suggesting that the carbonyl group on C(1) has formed a conjugated system with a double bond on C(2) and C(12).     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Novel Water Cluster [Mn(phen)_2·H_2O·Cl]·p-FBA·3H_2O

A novel water cluster [Mn(phen)2·H2O·Cl]·p-FBA·3H2O (p-FBA = p-fluorobenzoic acid and phen = 1,10-phenanthroline) was synthesized by the hydrothermal reaction of MnCl2 with p-FBA and phen at 150 ℃ and characterized by elemental analysis,IR spectra and TG. Its crystal structure was determined by X-ray single-crystal diffraction study. The crystal belongs to the triclinic system,space group P1,with a = 10.5768(1),b = 11.5960(1),c = 12.9916(2) ,α = 101.816(2),β = 95.397(2),γ = 103.052(2)o,V = 1502.8(3) 3,Z = 2,Dc = 1.463 g/cm3,R = 0.0399 and wR = 0.0997. The crystal structure shows that the manganese(Ⅱ ) ion is six-coordinated by four nitrogen atoms,one chloride ion and one oxygen atom forming a distorted octahedral coordination geometry. The structure includes three acyclically connected water molecules and one coordinated water molecule thus forming a (H2O)4 water cluster. This water pattern forms a cross-linked discrete ring. The steady (H2O)4 is further extended into a cage-like structure by the hydrogen-bonding interaction formed by dissociative aqua molecule and Cl-ligand. The dimer structure is further extended into a one-dimensional (1D) structure through C-H···O interaction. π···π Stacking interaction among adjacent phen aromatic rings further stabilizes the crystal structure.     

Synthesis and Crystal Structure of 12-（2,4-Dichlorophenyl）-7,8,9,10,11,12-hexahydrobenzo[f]pyrimido [4,5-b]quinoline-9,11-dione DMF Solvate

The title compound 12-(2,4-dichlorophenyl)-7,8,9,10,11,12-hexahydrobenzo-[f]pyrimido[4,5-b]quinoline-9,11-dione DMF solvate 1(C24H20Cl2N4O3,Mr=483.34) was synthesized and crystallized.The crystal belongs to the monoclinic system,space group P21/n with a=6.4798(16),b=20.595(5),c=16.723(4),β=95.267(7)o,Z=4,V=2222.3(9)3,Dc=1.445 g/cm3,μ(MoKα)=0.328 mm-1,F(000)=1000,the final R=0.0530 and wR=0.1388 for 3484 observed reflections(I2σ(I)).X-ray analysis reveals that the central 1,4-dihydropyridine ring is slightly distorted,adopting a half-chair conformation,which is obviously different from the boat conformations of other similar compounds.In addition,the classical hydrogen bonds of N(2)-H(2A)…O(2) are presented in the crystals,and link the adjacent molecules to form dimmers.Atom O(3) in the DMF solvent forms two hydrogen bonds of O(3)…H(1H)-N(1) and O(3)…H(3H)-N(3) with a pyrimidoquinoline moiety,forming an interesting half-chair-like conformation.The hydrogen bonds link the molecules to form dimmers,while intermolecular π-π interaction connects the above-mentioned dimmers to yield a one-dimensional structure.     

Synthesis and Crystal Structure of a New Complex [Cu（C_（14）H_9O_3）_2（C_5H_5N）_2（C_2H_5OH）_2]

The title compound of Cu(C14H9O3)2(C5H5N)2(C2H5OH)2(1) was synthesized via the hy- drothermal reaction of CuCl2·2H2O and 9-hydroxy-fluorene-9-carboxylic acid(HHF) with pyridine, and characterized by elemental analysis and infrared spectra. The crystal belongs to triclinic, space group P1 with a = 8.8302(12), b = 10.1625(14), c = 12.2708(17), α = 86.207(2), β = 69.562(2), γ = 64.932(2)o, V = 930.3(2) 3, Z = 1, Mr = 764.30, Dc = 1.364 g/cm3, F(000) = 399, S = 1.059 and μ(MoKα) = 0.644 mm-1. The final R = 0.0459 and wR = 0.1274 for 3414 observed reflections with I 2σ(I). The copper atom is six-coordinated by two oxygen atoms from two different 9-hydroxy-fluorene-9-carboxylate ligands, two pyridine nitrogen atoms and two ethanol oxygen atoms, forming a distorted octahedral coordination geometry. The extensive O–H···O hydrogen bonding connects the molecules to form a one-dimensional chain structure. Between adjacent one-dimensional chains, a two-dimensional layered structure was formed by fluorene ring π-π packing interaction. Between the layers, a three-dimensional structure was formed through the π-π packing interaction of the pyridine ring. Moreover, the thermal stability and photoluminescent property of the complex has been investigated.     

6,8-Di-tert-butyl-3-（2,4-dimethyl-quinolin-7-yl）-3,4-dihydro-2H-benzo[e][1,3]oxazine： Synthesis,Crystal Structure and Luminescent Properties

6,8-Di-tert-butyl-3-(2,4-dimethyl-quinolin-7-yl)-3,4-dihydro-2H-benzo[e][1,3]oxa- zine(1) was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3(C28 H35 Cl3 N2 O, Mr = 521.93) belongs to the triclinic system, space group P1 with a = 10.852(2), b = 11.352(2), c = 13.050(3), α = 101.95(3), β = 92.94(3), γ = 114.64(3)o, V = 1412.4(5)3, Z = 2, Dc = 1.227 g/cm3, F(000) = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725(I 2?(I)). The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H···O interactions, intermolecular C–H···N interactions, C–H···π interactions, and π···π interactions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.     

Synthesis, Crystal Structure and Quantum Chemistry of Tris[（2-methyl- 2-phenyl）propyl] （2,4-dinitro-phenolato）tin

The tris[(2-methyl-2-phenyl)propyl](2,4-dinitro-phenolato)tin was synthesized by the reaction of bis[tri(2-methyl-2-phenyl)propyltin] oxide with 2,4-dinitrophenol. The compound was characterized by IR, 1H NMR spectra and elemental analysis. The crystal structure has been determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/n with a = 0.9649(0), b = 1.0087(8), c = 3.4867(4) nm, β = 90.965(7) , Z = 4, V = 3.3933(7) nm3, Dc = 1.369 Mg·m-3, (MoKa) = 0.796 mm-1, F(000) = 1440, R = 0.0345 and wR = 0.0821. The tin atom has a distorted tetrahedral geometry. The 2D network structure of the complex is formed by hydrogen bonds and π-π effects. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of the complexes have been investigated with the aid of G98W software.     

Synthesis,Crystal Structure and Anion Recognition Property of a Flexible Urea-functionalized Receptor

A flexible urea-functionalized receptor bearing two p-nitrobenzene units was designed and synthesized from the reaction of precursors 4-nitrophenyl isocyanate and 1,2-bis(2?-aminophenoxy) benzene. The receptor was characterized by ~1 H NMR, MS, FTIR and elemental analysis, and the crystal structure of the receptor was determined by X-ray diffraction analysis. The crystal belongs to the orthorhombic system, space group Pca21 with a = 12.740(2), b =14.133(3), c = 15.842(3) ?, V = 2852.4(9) ?~3, Z = 4, M_r = 620.57, D_c = 1.445 g/cm~3, F(000) = 1288,= 0.0585 and wR = 0.1032 for 3177 observed reflections(Ⅰ 2σ(Ⅰ)), and R = 0.1304 and wR =for all data. The results show that the receptor displays selective recognition ability for H_2PO_4~– in DMSO with a series of anions using UV-Vis absorption spectra technique. Furthermore, the coordination reaction of the receptor with H_2PO_4~– was investigated via UV-Vis spectra and ~1 H NMR.The stoichiometric ratio and the association constant(Ka) of the coordination reaction were obtained as well.     

Crystal and Molecular Structure of Guanidinium Pentamolybdobis (n-amylphosphonate)(CN3H6)4[(n-C5H11P)2Mo5O21]

The crystal structure of guanidinlum pentamolybdobis(n-ainylphcsphonate), which contains the longest carbon chain hitherto known, was determined by single-crystal X-ray diffraction analysis. It belongs to monoclinic, space group C2/c, Z = 4, 0=18.857(2), b=12.170(1), c=18. 294(2) A .β=102.73 (2), V=4095. 2A3.u= 140. 34 cm-1. The intensity data were collected on an Enraf-Nonius CAD4 diffractometer with MoKa radiation. The positions of all molybdenum and phosphorus atoms were determined by the direct method. The other non-hydrogen atoms were revealed by difference Fourier synthesis. The structure was refined by full-matrix least-squares procedure to a final R value of 0. 068. The structure of the anion is similar to [(CH2P)2Mo5O21]4-, [(NH3C2H4P)2Mo6O21]2-, [(n-C3H7As)2Mo5O21]--, and [(C3H5As)2Mo6O21]4-. It consists of a ring of five distorted MoO, octahedra joined by edge-sharing, except for one pair which is joined by corner- sharing. The size of the Mo6O16 ring is close to those of [(CH3P)2Mo5O21]4- a     

Synthesis and Crystal Structure of [K（2,2,2-crypt）]_3Sb_（11）

The title complex [K(2,2,2-crypt)]3Sb11 has been prepared by the reaction of K3Cd2Sb with Cu-C≡CH in ethylenediamine in the presence of 2,2,2-crypt, and characterized by low temperature X-ray structure analysis. The crystal is of orthorhombic system, space group C2221 with a = 15.475(3), b = 22.807(5), c = 24.834(6), V = 8765(3)3, Dc = 1.960 g/cm3, C54H108K3N6O18Sb11, Mr = 2586.01, F(000) = 4944, μ = 3.531 mm-1, Z = 4, R = 0.0442 and wR = 0.1053 for 10265 observed reflections (I > 2σ(I)). The "naked" Sb113- anion is stable due to the completely sequestered alkali metal cations through ion-ion interactions.     

Synthesis and Crystal Structure of 2-Oxo-3-phenyl-1-oxaspiro[4.5]dec-3-en-4-yl 4-chlorobenzoate

The title compound 2-oxo-3-phenyl-1-oxaspiro[4.5]dec-3-en-4-yl 4-chloro-benzoate 6 (C22H19ClO4, Mr = 382.82) has been synthesized by the condensation reaction of 4-hydroxy-3-phenyl-1-oxaspiro[4.5]dec-3-en-2-one 5 with 4-chlorobenzoyl chloride, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/n with a = 10.6749(11), b = 6.0573(7), c = 29.680(2) , β = 94.073(3)o, V = 1914.3(3) 3, Z = 4, Dc = 1.328 g/cm3, F(000) = 800, μ = 0.224 mm–1, S = 1.003, the final R = 0.0605 and wR = 0.1500 for 1828 observed reflections with I > 2σ(I) and 244 variable parameters. The crystal analysis shows that the molecular structure of the title compound has one planar furan ring, one chair conformation cyclohexane ring and two benzene rings. The furan and cyclohexane rings adopt whorl conformations.     

Synthesis and Crystal Structure of N-phenyl-N-[（o-nitrophenylacetyl）oxy]benzamide

The compound N-phenyl-N-[（o-nitrophenylacetyl）oxy]benzamide （C21HI6N2Os, Mr = 376） has been synthesized by the reaction of N-hydroxy-N-phenylbenzamide with 2-（2-nitro- phenyl）acetyl chloride in dichlorom-ethane and its structure Was characterized by 1H NMR, 13C NMR, IR, H RMS（ESI） and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 32.30（2）, b = 8.400（5）, c = 15.099（9） A, fl = 114.256（10）°, V = 3735（4） A3, Z = 8, D, = 1.339 g/cm3, F（000） = 1568, p = 0.097 mm-1, the final R = 0.0506 and wR = 0.1176 for 2318 observed reflections （1 〉 2a（/））. The title molecule contains three branched chains with its center placed at the midpoint of N. The phenyl ring （C（1）＇-C（6）） makes a dihedral angle of 70.3（1）° with the phenyl ring （C（10）-C（15）） of benzoyl group, and 14.3（1）° with the phenyl ring （C（16） - C（21））, Hydrogen bonds C（5）-H（5）...O（1） and C（12）-H（12）...O（3） together with it-Jr stacking interactions contribute to the stability of the structure.     

苯四甲酸桥连的镍配合物[Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O的合成及结构

At room temperature, a coordination polymer [Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O was synthesized by reaction of NiCl2·6H2O, 1,2,4,5-benzenetetracarboxylic dianhydridc and imidazole in a water/THF solution. The structure was determined by X-ray diffraction crystal structure analysis. It crystallizes in triclinic P1 space group with the crystal cell parameters of a=0.67542 (2) nm, b=1.000 14 (1) nm, c=1.09088 (3) nm, α=74.140(2)°, β= 74.388(1)°, y=73.239(2)°, and V=0.664 09(3) nm3, Z=1. The crystal structure shows that Ni1 atom is coordinated by four water and two imidazole molecules, while Ni2 is coordinated by four water molecules and two carboxyl oxygen atoms. The 1,2,4,5-benzenetetracarboxylate ions bridge Ni2 coordination centers to form one-dimensional chain structure. Moreover, the chains are further linked together by hydrogen bonds to form a two-dimensional network. CCDC: 295873.