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1.
The title compound, ethyl 2-(4-methoxyphenyl)-1H-benzo[d]imidazole-5-carboxylate dihydrate (5), was synthesized and its crystal structure was studied by single-crystal X-ray diffraction technique. Compound 5 is crystallized in the centrosymmetric triclinic space group \(P\bar {1}\) with Z?=?4 and Z′?=?2, and unit-cell parameters of a?=?8.9190 (3) Å, b?=?12.6888 (4) Å, c?=?14.7111 (5) Å, α?=?98.4855 (10)°, β?=?101.6379 (9)°, γ?=?95.4346 (10)° and V?=?1599.43 (9) Å3. Its starting material, 4-fluoro-3-nitrobenzoic acid (1), is crystallized in the non-centrosymmetric monoclinic space group P21 and Z?=?4 with unit-cell parameters of a?=?3.7170 (4) Å, b?=?12.6475 (13) Å, c?=?15.5237 (15) Å, α?=?90°, β?=?91.9786 (16)°, γ?=?90° and V?=?729.35 (13) Å3. It was noted that strong hydrogen bonds play important roles in the crystal packing of both compounds, especially in 5, in which the co-crystallized water molecules act as both strong hydrogen bond donor and strong hydrogen bond acceptor.

Graphical Abstract

Two molecule of compound 5 crystallized in a non symmetrical manner with four co-crystallized water molecules which play an important role in the crystal packing as strong hydrogen-bond donors.
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2.
The reaction of the potentially bidentate ambidentate N,O-donor ligands 3-hydroxy-2-pyridinecarboxylic acid (Hhpc) and 3-hydroxy-2-(hydroxymethyl)pyridine (Hhhp) with trans-[ReOCl3(PPh3)2] led to the isolation of the products [ReOCl(hpc)2] (1) (from acetonitrile) and [ReOCl2(hhp)(PPh3)] (2) (from ethanol) respectively. In both complexes hpc and hhp are coordinated as bidentate N,O-donor chelates, rather than as O,O-donor ligands. From the reaction of [Re(CO)5Cl] and Hhhp·HCl in ethanol the neutral complex fac-[Re(CO)3Cl(Hhhp)] (3) was obtained, with N,O-coordination of Hhhp. Complex 1 crystallizes in the monoclinic space group P21/n with a?=?6.8782(3), b?=?20.0647(8), c?=?10.8692(4) Å, β?=?107.545(1)°, and Z?=?4. Complex 2 crystallizes in the triclinic space group P-1 with a?=?7.3523(4), b?=?8.1047(5), c?=?19.591(1) Å, α?=?91.133(2)°, β?=?93.656(2)°, γ?=?93.074(2)° and Z?=?2. Complex 3 has monoclinic P21/c symmetry with the cell parameters a?=?10.6452(5), b?=?11.1372(5), c?=?9.7229(5) Å, β?=?106.107(2)°, and Z?=?4.

Graphical Abstract

The reaction of the potentially bidentate ambidentate N,O-donor ligands 3-hydroxy-2-pyridinecarboxylic acid (Hhpc) and 3-hydroxy-2-(hydroxymethyl)pyridine (Hhhp) with trans-[ReOCl3(PPh3)2] led to the isolation of the products [ReOCl(hpc)2] (from acetonitrile) and [ReOCl2(hhp)(PPh3)] (from ethanol) respectively. In both complexes hpc and hhp are coordinated as bidentate N,O-donor chelates, rather than as O,O-donor ligands. From the reaction of [Re(CO)5Cl] and Hhhp·HCl in ethanol the neutral complex fac-[Re(CO)3Cl(Hhhp)] was obtained, with N,O-coordination of Hhhp. Spectroscopic data and the X-ray crystal structures of the complexes are reported.
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3.
2-amino-3-ethoxycarbonyl-4-(4′-methoxy Phenyl)-4H-pyrano-[3,2-c]-chromene-6-methyl-5-one was synthesized by the two-component reaction of 6-methyl-4-hydroxy coumarin with 4′-methoxy-2-cyano cinnamate, which was synthesized by Knoevenagel reaction with 88% yield. The compound obtained was characterized by spectroscopic techniques and confirmed by X-ray crystallographic studies. The crystallographic data analysis reveals that the title compound crystallizes in the triclinic space group \(P\overline{1}\) with cell parameters a = 7.7750(8) Å, b = 9.0310(6) Å, c = 15.6120(17) Å, α = 77.249(7)°, β = 115.860(3)°, γ = 70.139(7)°, V = 1,003.0(16) Å3 for Z = 4. The structure has been solved by direct methods and refined to R1 = 0.0552 for 3,164 observed reflections with I > 2 σ(I). The pyran ring is in a flattened boat conformation. The carbonyl group is oriented in a -synperiplanar(cis) conformation.
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4.
9-(4-Nitrophenyl)-3,3,6,6-tetramethyl-3,4,6,7,9,10-hexahydro-1,8(2H,5H) acridinedione (NTHA) crystallizes in orthorhombic space group P212121 with a = 5.9716(1) Å, b = 18.0476(3) Å, c = 19.2445(2) Å, V = 2074.04(5) Å3, Z = 4, Dcal = 1.263 Mg m?3 and R = 0.0521 (wR = 0.1326) for 4078 observed reflections. 9-(4-Nitrophenyl)-10-(4-methoxyphenyl)-3,3,6,6-tetramethyl-3,4,6,7,9,10-hexahydro-1,8(2H,5H) acridinedione NMTHA, crystallizes in monoclinic space group P21/c with a = 15.669(5) Å, b = 10.652(4) Å, c = 18.337(6) Å, β = 108.25(1)°, V = 2906.66(2) Å3, Z = 4, Dcal = 1.245 Mg m?3 and R = 0.0725 (wR = 0.1847) for 5105 observed reflections. The experimental values are compared with the theoretical values calculated based on the semiemperical methods. The structures are stabilized by N–H?sO and C–H?sO types of intermolecular interactions in addition to van der Waals forces.  相似文献   

5.
1-[(E)-2-(4-bromophenyl)-1-diazenyl]-3-({3-[(E)-2-(4-bromophenyl)-1-diazenyl]-6-ethylhexahydro-1-pyrimidinyl}methyl)-4-ethylhexahydropyrimidine (1) has been synthesized by reaction of a mixture of formaldehyde and 1,3-pentanediamine{DYTEK®EPdiamine} with p-bromobenzenediazonium chloride. This compound crystallizes in two polymorphic forms 1-α and 1-β whose crystal structures have been determined by single crystal X-ray diffraction analysis. Both polymorphs 1-α and 1-β display crystallographic disorder within the hexahydropyrimidine rings. The molecule of 1 is built up of two equivalent 3-(aryldiazenyl)-6-ethylhexahydro-1-pyrimidinyl groups in the s-trans orientation around the central methylene group (C13). In both structures the triazene moieties adopt the anti configuration around the N=N bonds, displaying significant π-conjugation. The crystal packings are determined only by van der Waals interactions. The crystal structures of 1-α and 1-β are compared with the previously reported structure of the 5,5-dimethylhexahydropyrimidine analogue 3. Compounds 1 and 3 are isomeric with respect to the hexahydropyrimidine moiety. The structures of 1 and 3 are very different in one respect; in 1 the aryldiazenyl-hexahydropyrimidinyl groups are in the s-trans orientation around the central methylene group, whereas in 3 the arrangement of the aryldiazenylhexahydropyrimidinyl groups is the s-cis orientation. Crystal data: 1-α C25H34N8Br2, monoclinic, space group P2(1)/c, a = 9.2150(3), b = 19.4059(6), c = 15.4324(5) Å, β = 98.738(1)°, V = 2727.7(2) Å3, for Z = 4; 1-β C25H34N8Br2, triclinic, space group P-1, a = 9.6009(3), b = 10.7509(4), c = 14.2169(5) Å, α = 99.830(2), β = 105.973(3), γ = 95.578(1)°, V = 1373.9(1) Å3, for Z = 2.  相似文献   

6.
The molecular and crystal structures of the 4-hydroxy derivative of (3R,6R)-3-methyl-6-isopropyl-2-(4-phenylbenzylidene)cyclohexanone are determined by X-ray diffraction analysis. Single crystals are orthorhombic, a = 9.147(2) Å, b = 12.959(2) Å, c = 15.695(5) Å, V = 1860.4(7) Å3, Z = 4, and space group P212121. The cyclohexanone ring in the crystal structure has an asymmetric chair conformation. The puckering parameters are as follows: the puckering amplitude S is 0.91, and the puckering angles θ and ψ are equal to 20.2° and 10.4°, respectively. It is established that the enone fragment and the cyclohexanone ring in molecules are flattened considerably. In the crystal structure, the molecules are linked by the
hydrogen bonds (bond length, 1.85 Å). The structural features and the strength of the hydrogen bonds for the compound under investigation and its analogue with one benzene ring are compared using the X-ray diffraction and IR spectroscopic data.
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7.
[1,2,3-13C3]-1-(Phenylsulfinyl)-3-benzyloxyacetone, C16H16O3S, (3) has been synthesized and its crystal structure has been determined by a single-crystal X-ray diffraction analysis. The X-ray diffraction study revealed that compound 3 crystallizes in the monoclinic crystal system in the acentric space group Pc, with cell constants at T = 100 K: a = 16.073(5), b = 5.5079(16), c = 7.949(2) Å, β = 100.221(4)°, V = 692.6(3) Å3, Z = 2, d calc = 1.383 g/cm3. Compound 3 contains the chiral tetravalent three-coordinated sulfur atom, which has a distorted tetrahedral configuration with a lone electron pair occupying one of the tetrahedron vertices. In the crystal, the molecules are packed in stacks along the b axis; the stacks consist of the molecules of the same chirality. Furthermore, the stacks of the molecules of the opposite chirality alternate along the c axis. The molecules in neighboring stacks are arranged by head-to-tail orientations. There are no short intermolecular contacts in the crystal of 3.  相似文献   

8.
The crystal structure of 2,3H-2-methyl-4-(4-nitrophenyl)-5-oxobenzopyrano[3,4-e]dihydropyran-2-ol is investigated using X-ray diffraction. The unit cell contains an ethanol molecule that forms hydrogen bonds with O-H and C-O groups of two molecules of the main compound and acts as a proton donor and a proton acceptor in these hydrogen bonds. Owing to these interactions, infinite chains are formed in the crystal. The crystallographic data for the structure of C19H15NO6·C2H5OH (M = 399.39) are as follows: the crystals are triclinic, space group P1, a = 5.5340(3) Å, b = 8.0109(4) Å, c = 11.0112(5) Å, α = 88.773(2)°, β = 84.788(2)°, γ = 79.958(2)°, and Z = 1.  相似文献   

9.
(4E)-5-(3-Chlorophenyl)-N-(4-chlorophenyl)-2-diazo-3-oxopent-4-enoic acid amide (5) was synthesized from p-chloroaniline to N-(4-chlorophenyl)-2-diazo-3-oxo-butyramide (4) with 3-chlorobenzaldehyde. The yielded product 5 was investigated with X-ray crystallographic, NMR, MS, and IR techniques. Compound 5 (C17H11Cl2N3O2, Formula wt = 360.19), crystallizes in the monoclinic space group P21/c with unit cell parameters a = 10.516(2), b = 17.996(4), c = 8.902(2) Å, α = 90.00, β = 105.36(3), γ = 90.00°. V = 1624.5(6) Å3, Z = 4, D x = 1.473 Mg m?3. The final R was 0.0511.  相似文献   

10.
The solid state structure of an N-heterocyclic borane 1,1,3,3-tetramethyl-1,3λ4,2-diazaborolidin-1-ium chloride is reported. This molecule features numerous Cl?H hydrogen bonds.

Graphical Abstract

The crystal structure of 1,1,3,3-tetramethyl-1,3λ4,2-diazaborolidin-1-ium chloride shows multiple C–H?Cl interactions in the solid state.
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11.
A series of new coordination compounds has been synthesized using the organic ligand 1,2-dimethoxy-4,5-bis(2-pyridylethynyl)benzene (dmpeb). The compounds all form dimers consisting of two metal cations bridged by two ligand molecules. Charge balance is provided by halide ligands, and the four-coordinate metal centers are distorted from the ideal tetrahedral environment. [CoCl2(dmpeb)]2 (1) crystallizes in the monoclinic space group P21/n with a = 8.5272(6) Å, b = 18.3653(13) Å, c = 13.3493(9) Å, β = 103.574(2)°, V = 2032.2(2) Å3, Z = 2. [ZnCl2(dmpeb)]2 (2) is isostructural to 1 and has the cell parameters a = 8.5495(4) Å, b = 18.4049(8) Å, c = 13.3692(6) Å, β = 103.4460(10)°, V = 2046.01(16) Å3, Z = 2. [ZnBr2(dmpeb)]2 (3) is also isostructural to 1 with a = 8.7882(5) Å, b = 18.7260(12) Å, c = 13.3857(8) Å, β = 102.5990(10)°, V = 2149.8(2) Å3, Z = 2. Additionally, the compounds [ZnI2(dmpeb)]2 (4, cell parameters: a = 8.9650(5) Å, b = 19.1251(10) Å, c = 13.4160(7) Å, β = 101.1660(10)°, V = 2256.7(2) Å3, Z = 2), [HgCl2(dmpeb)]2 (5, cell parameters: a = 8.8457(7) Å, b = 18.4030(15) Å, c = 13.3711(11) Å, β = 104.246(2)°, V = 2109.7(3) Å3, Z = 2), and [HgBr2(dmpeb)]2 (6, cell parameters: a = 9.0576(5) Å, b = 18.8634(11) Å, c = 13.4535(8) Å, β = 102.9780(10)°, V = 2239.9(2) Å3, Z = 2) are also isostructural to 1. A seventh dimeric compound, [HgI2(dmpeb)]2, not isostructural to the others was also characterized by X-ray crystallography. [HgI2(dmpeb)]2 (7) crystallizes in the triclinic space group P-1 with a = 8.8028(5) Å, b = 12.0990(7) Å, c = 12.4082(7) Å, α = 109.7240(10)°, β = 107.3680(10)°, γ = 93.0880(10)°, V = 1169.57(12) Å3, Z = 1.  相似文献   

12.
The crystal structure of 2-[(4-nitrophenyl)carbonyl]cyclohex-1-ene-1-yl 4-nitrobenzoate is studied (T = 173 K, R1 = 0.0354 for 2713 observed reflections). This crystal is orthorhombic, a = 7.8367(8) Å, b = 9.6082(10) Å, c = 23.856(3) Å, V = 1796.3(3) Å3, space group P212121, and Z = 4. The molecule has a folded configuration, which is stabilized by π-π interactions between its two parts. A system of intermolecular C-H...O hydrogen bonds (H...O, 2.44–2.67 Å; CHO angles 122°–169°) and intramolecular C-H...O contacts closing five-membered cycles (H...O, 2.42–2.59 Å; CHO angles 96°–102°) are formed in the structure.  相似文献   

13.
A novel two-dimensional coordination polymer [Ag(μ3-hexamethylenetetramine)(H2O)](BF4) was synthesized and characterized by X-ray crystallography. It crystallized in the orthorhombic space group Pnnm with a = 15.561(7) Å, b = 10.754(5) Å, c = 6.514(3) Å, and Z = 4. Each Ag center is four-coordinated in a slightly distorted tetrahedral geometry. The structure consists of 2D wavy layers of hexagonal units; these 2D layers are further connected to form a 3D network by O-H⋯F, C-H⋯F hydrogen bonds with counter anions BF 4 in the layers. From Kristallografiya, Vol. 50, No. 4, 2005, pp. 648–650. Original English Text Copyright ? 2005 by Kong, Zhang, Sun, Okamura, Ueyama. The text was submitted by the authors in English.  相似文献   

14.
The crystal structure of the title compound has been determined. The compound crystallizes in the monoclinic space group P21/c with a = 5.9885(2) Å, b = 14.7345(4) Å, c = 12.3719(4) Å, β = 96.655(5)°, V = 1084.31(8) Å3, z = 4. An intramolecular N–H···N hydrogen bond forms a pseudo-six-membered ring with graph set S 1 1(6). The crystal structure is stabilized by intermolecular interactions of the type N–H···N and C–H···N. The packing motifs in accordance with Etter’s analysis are R 2 2(8) corresponding to N–H···N dimer and that generated by the chain is C(7).  相似文献   

15.
The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C15H11N3O2S2 · C3H7NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P21/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.  相似文献   

16.
A water soluble compound, (2-((1H-benzimidazol-2-yl)methylamino)acetic acid, BIGH, has been synthesized and structurally characterized by elemental analysis, IR and UV spectroscopies, 1H-NMR, thermogravimetric and differential thermal analyses, and single crystal and powder X-ray diffraction. BIGH can act as a flexible planar ligand with three potential coordination sites. It crystallizes in a monoclinic system with the sp. gr. P21/c with the unit cell parameters, a = 9.3764(7) Å, b = 11.5031(8) Å, c = 10.0543(6) Å, and Z = 4. The crystal structure was stabilized through inter-molecular hydrogen bonds. The anti-microbial activity of the compound has been studied against Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, and Staphylococcus aureus, which showed a good activity against Bacillus subtilis. Cyclic voltammogram of the compound shows that it is a redox-active molecule.  相似文献   

17.
The crystal structure of 4-phenylquinolin-2-(1H)-one (C15H11NO) is determined by X-ray diffraction. The compound crystallizes in the orthorhombic crystal system (space group Pbca) with the unit cell parameters a = 7.382(2) Å, b = 21.795(3) Å, c = 14.066(5) Å, and Z = 8. The structure is solved by direct methods and refined to an R-value of 0.0398 for 1360 observed reflections [F0 > 4σ (F0)]. The quinoline moiety and the substituted phenyl ring are nearly planar. The dihedral angle between these two moieties is 64.65(6)°. The crystal structure is stabilized by two intermolecular N-H?O and C-H?O interactions.  相似文献   

18.
The structure of 1-(4-chlorophenacyl)-4-methyl-1,5,6,7-tetrahydro-2H-cyclopenta[b]pyridin-2-one is studied using single-crystal X-ray diffraction. The structure (a = 37.006(8) Å, b = 8.967(3) Å, c = 27.911(3) Å, β = 96.52(2)°, Z = 24, space group P21/c) is solved by direct methods and refined to R1 = 0.0608 and wR2 = 0.1170. Six crystallographically independent molecules differ in the dihedral angle between the phenyl and heterocycle planes. The formation of Cl?Cl aggregates is discussed.  相似文献   

19.
Bis(acetylacetonato)oxovanadium C10H14O5V (I) and (S)-[2-(N-salicylidene)aminopropionate]oxovanadium monohydrate C10H9NO5V (II) are synthesized. The crystal structures of compounds I and II are determined using single-crystal X-ray diffraction. Crystals of compound I are triclinic, a = 7.4997(19) Å, b = 8.2015(15) Å, c = 11.339(3) Å, α = 91.37(2)°, β = 110.36(2)°, γ = 113.33(2)°, Z = 2, and space group \(P\bar 1\). Crystals of compound II are monoclinic, a = 8.5106(16) Å, b = 7.373(2) Å, c = 9.1941(16) Å, β = 101.88(1)°, Z = 2, and space group P21. The structures of compounds I and II are solved by direct methods and refined to R1 = 0.0382 and 0.0386, respectively. The oxovanadium complexes synthesized are investigated by vibrational spectroscopy.  相似文献   

20.
The title compound is crystallized in the monoclinic space group P21/c with cell parameters a = 7.499, b = 13.336, c = 19.390 Å, β = 99.716°, V = 1911.4 Å3, Z = 4, D cal = 1.273 Mg/m3 at T = 120 K. The structure is refined by full-matrix least-squares procedures to final R 1 = 0.0548 and wR 2 = 0.1089 for 3424 reflections. Two phenyl rings are noncoplanar with regard to each other and pyrrolidine core. The structure contains intramolecular hydrogen bond.  相似文献   

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