共查询到20条相似文献,搜索用时 31 毫秒
1.
Abstract The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ = 90.00o. V = 949.6(3) ?3, Z = 4, Dx = 1.665 Mg m−3. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?3, Z = 8, D
m = 1.304 Mg m−3. The final R was 0.0565.
Index Abstract The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ =90.00o. V = 949.6(3) ?3, Z = 4, Dx = 1.665 Mg m−3. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?3, Z = 8, D
m = 1.304 Mg m−3. The final R was 0.0565.
相似文献
2.
Heng-Shan Dong Yan-Fei Wang Hong-Ru Dong Bin Wang Bin Quan 《Journal of chemical crystallography》2009,39(2):91-94
Abstract The N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide 6 was synthesized from aryl triazole acids and its structure is established by MS, IR, and 1H NMR spectral data. Compound 6, C22H22N8O4, Mr = 462.48, crystallizes in the monoclinic space group P2(1)/c with unit cell parameters a = 15.3451(8), b = 8.6486(4),
c = 16.8502(9) ?, α = 90.00, β = 95.731(2), γ = 90.00o, V = 2225.1(2) ?3, Z = 4, and Dx = 1.381 mg m−3. The final R was 0.0450. The four aromatic rings are close to linear because of N···H–N hydrogen bonds.
Index Abstract Synthesis and crystal structures of N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide
Heng-Shan Dong, Yan-Fei, Wang, Hong-Ru Dong, Bin, Wang, Bin Quan
N,N′-Bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide was synthesized.
相似文献
3.
Abstract The title compound bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol 8 has been synthesized and established by H NMR, IR and MS spectra and X-ray diffraction crystallography. Compound 8, C23H29Cl2N3O, Mr = 424.31, crystallizes in the monoclinic space group P21/c with unit cell parameters a = 14.5402(6) ?, b = 12.5888(5) ?, c = 11.6510(5) ?, α = 90o, β = 100.183o(2), γ = 90o, V = 2099.05(15) ?3, Dx = 1.343 mg m−3 and Z = 4. The final R was 0.0514. The molecular conformation and packing is stabilized by interactions of intermolecular
O1–H1···N3′.
Index Abstract The structure of bis(3-chlorophenyl)-[5-methyl-1-(4-methylphenyl)-1,2,3-triazol-4-yl]-methanol by the reaction of compound
4 and Grignard regent is studied.
相似文献
4.
Abstract The 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester 6 was synthesized from p-bromoaniline. The yielded product 6 was investigated with X-ray crystallographic, NMR, MS, and IR techniques. Compound 6, C13H15BrN4O2S, Mr = 371.26, crystallizes in the monoclinic space group P21/n with unit cell parameters a = 5.5220(1), b = 26.996(5), c = 10.596(2) ?, β = 103.83(3). V = 1533.8(5) ?3, Z = 4, Dx = 1.608 mg m−3. The final R
1 was 0.0844; wR
2 was 0.1560. H-bond is discussed.
Index Abstract The structure of 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester from 5-amino-1-(4-bromophenyl)-1,2,3-triazol-4-carboxylic acid ethyl ester is
studied. H-bond is discussed.
相似文献
5.
S. Rajeswari G. Venkatesa Prabhu D. Tamilvendan V. Ramkumar 《Journal of chemical crystallography》2009,39(9):650-654
Abstract A new mannich base 1-[(2,5-dioxopyrrolidin-1-yl)(phenyl)methyl] thiourea formed by the direct condensation of thiourea, succinimide
and benzaldehyde has been synthesized. The structure of this mannich base has been elucidated on the basis of micro elemental
analysis, IR, 1H NMR, 13C NMR, Mass and UV–Visible Techniques. The crystal structure of the title compound C12 H13 N3 O2 S was determined. It crystallizes in the monoclinic system, space group P21/c with a = 10.8234 (7) ?, b = 6.0355 (5) ?, c = 19.3692 (14) ?, β = 100.540(3)°, Z = 4 and V = 1243.94 (16) ?3. The structure was solved by the full-matrix least squares on F
2 and had a refined R value of 0.0465 for 1,964 observed reflections. The crystal structure is stabilized by strong intramolecular C–H···O, C–H···S
interactions and inter molecular N–H···O and S···S interactions.
Graphical Abstract This paper describes the spectroscopic and crystallographic studies of the title compound which is essential in ascertaining
the structure of this new compound.
相似文献
6.
Arzu Özek Çiğdem Albayrak Mustafa Odabaşoğlu Orhan Büyükgüngör 《Journal of chemical crystallography》2009,39(5):353-357
Abstract The crystal structure of C14H12ClNO2 was determined by X-ray analysis. It crystallizes in the triclinic space group Pc with a = 12.5346(10) ?, b = 4.5101(3) ?, c = 12.0534(11) ?, α = 90.00o, β = 113.669(6)o, γ = 90.00o, Z = 2, Dx = 1.393 mg/m3, μ (MoKα) = 0.298 mm−1. The title compound is photochromic and molecule is non-planar. It adopts a phenol–imine tautomeric form with a strong intramolecular
O–H···N hydrogen bond and a strong intermolecular C–H···O hydrogen bond. Minimum energy conformations AM1 were calculated
as a function of the three torsion angles θ1(C10–C9–N1–C8), θ2(C9–N1–C8–C1) and θ3(N1–C8–C1–C6), varied every 10°. As in the X-ray experiment results, molecule has an angle that makes it non-planar between
two aromatic rings in AM1 optimized geometry.
Graphical Abstract Molecular and crystal structure of [(E)-2-[(3-chlorophenylimino)methy])-4-methoxyphenol], C14H12ClNO2, have been determined by single crystal X-ray diffraction study, and conformational analysis of the title molecule with respect
to the selected torsion angle has been achieved by AM1 semi-empirical calculations.
相似文献
7.
Hande Petek Çiğdem Albayrak Mustafa Odabaşoğlu İsmet Şenel Orhan Büyükgüngör 《Journal of chemical crystallography》2008,38(12):901-905
Abstract The single crystal X-ray diffraction analysis of the title compound, C15H15NO3, shows that the structure is adopted to its NH tautomeric form and crystallizes in the orthorhombic space group P bcn with a = 21.2424(15) ?, b = 12.7696(9) ?, c = 9.3605(10) ?, Z = 8, V = 2539.1(4) ?3, D
c
= 1.346 g/cm3. The molecular conformation in the crystal is stabilized by an intramolecular H-bond and the crystal structure is stabilized
by the bifurcated O–H···O type intermolecular H-bonds. In order to understand the effects on conformational flexibility of
the title molecule, molecular energy profile was calculated as a function of the selected torsion angle by means of AM1 semi-empirical
method.
Index Abstract Molecular and crystal structure of [(Z)-2-ethoxy-6-[(2-hydroxyphenylamino)methylene]cyclohexa-2,4-dienone], C15H15NO3, have been determined by single crystal X-ray diffraction study, and conformational analysis of the title molecule with respect
to the selected torsion angle has been achieved by AM1 semi-empirical calculations. 相似文献
8.
Abstract A pair of CuII coordination isomers [Cu(pmt)2] · 4H2O (1) and {[Cu(pmt)2] · 2H2O}
n
(2) [Hpmt = 2-(2-pyridylmethylamino) ethanesulfonic acid] have been prepared by reaction of the same proportion CuCl2 · 2H2O and Hpmt but with different experimental methods in water–methanol mixed solution, and were characterized by X-ray diffraction,
elemental analysis, IR spectrum. X-ray analysis indicates that complex (1) is a mononuclear complex in which two deprotonated pmt ligands coordinate in a facial tridentate arrangement about the CuII atom. While complex (2) is a coordination polymer, in which four N atoms of pmt ligands coordinate to one CuII atom but its sulfonate O atoms bond to adjacent CuII atom. Thus 12-membered rings (–Cu–N–C–C–S–O–)2 are obtained between two neighbouring CuII atoms and they connect one another to form this new polymer. Crystal data: [Cu(pmt)2] · 4H2O (1), Mr = 566.10, monoclinic, P2
1/c, a = 9.1950(8) ?, b = 11.5093(10) ?, c = 11.2304(10) ?, β = 105.5550(10)°, Z = 2, V = 1144.96(17) ?3, R
1
= 0.0407, wR
2
= 0.1242 [I > 2σ (I)]; {[Cu(pmt)2] · 2H2O}
n
(2), Mr = 530.07, triclinic, P-1, a = 7.6165(19) ?, b = 8.806(2) ?, c = 9.592(4) ?, α = 104.933(4)°, β = 106.732(4)°, γ = 109.503(3)°, Z = 1, V = 534.2(3) ?3, R
1 = 0.0470, wR
2 = 0.1082 [I > 2σ(I)].
Index Abstract A pair of CuII coordination isomers [Cu(pmt)2] · 4H2O (1) and {[Cu(pmt)2] · 2H2O}
n
(2) [Hpmt = 2-(2-pyridylmethylamino) ethanesulfonic acid] have been prepared by reaction of the same proportion CuCl2 · 2H2O and Hpmt but with different experimental methods in water–methanol mixed solution.
相似文献
9.
Abstract The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C17H19NO4, M
r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal
belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.3870(10), c = 17.780(2) ?, β = 91.102(2)°, V = 1557.4(3) ?3, Z = 4, D
c = 1.285 g/cm3, λ = 0.71073 ?, μ(Mo Kα) = 0.092 mm−1, F(000) = 640. The final refinement gave R = 0.0452, wR(F
2) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure
is stabilized by C–H···O, O–H···O and O–H···N hydrogen bonds and π–π stacking interactions.
Graphical Abstract The title compound 2-(2,3,4-trimethoxy-6-methylbenzylideneamino)phenol (C17H19NO4, M
r = 301.33) was synthesised and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal
belongs to monoclinic, space group P21/c, with a = 10.4458(14), b = 8.387(1), c = 17.780(2) ?, β = 91.102(2)°, V = 1557.4(3) ?3, Z = 4, D
c = 1.285 g/cm3, λ = 0.71073 ?, μ(Mo Kα) = 0.092 mm−1, F(000) = 640. The final refinement gave R = 0.0452, wR(F
2) = 0.1065 for 2,743 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the molecule adopts an E configuration at the C=N functional bond. The dihedral angle between the two phenyl rings is 38.3(3)°. The crystal structure
is stabilized by C–H···O and O–H···O hydrogen bonds and π–π stacking interactions.
相似文献
10.
Abstract The zinc(II) complex with 2-(2-hydroxyphenyl)benzimidazole, namely [Zn(2-(2-hydroxyphenyl)benzimidazolate)2]·C2H5OH (1 · C2H5OH) has been synthesized and characterized by X-ray crystallography and photoluminescent analysis. The complex crystallizes
in monoclinic space group P21/c with cell parameters a = 10.156(1) ?, b = 25.771(3) ?, c = 9.674(1) ?, α = 90°, β = 103.641(2)°, γ = 90°, Z = 4, V = 2460.4(4) ?3. The central Zn(II) is four-coordinate and has a tetrahedral geometry. The steady-state and time-resolved photoluminescent
spectra for the title compound have also been studied. The emission property can be ascribed to ligand-centered charge-transfer
transition (LCCT) with π → π* property.
Index Abstract
A new co-crystal of Zn(II) complex of 2-(2-hydroxylphenyl)benzimidazole with ethanol solvate has been prepared, characterized
by X-ray crystallography and fluorescent studies.
相似文献
11.
Irena Ćaleta Dominik Cinčić Grace Karminski-Zamola Branko Kaitner 《Journal of chemical crystallography》2008,38(10):775-780
Abstract Two novel benzothiazoles 2-chloro-N-(benzothiazol-2-yl)benzamide (1) and 2-chloro-N-(6-cyanobenzothiazol-2-yl)benzamide (2) were obtained in multistep synthesis. They were characterised by means of IR, 1H- and 13C-NMR spectroscopy and also by single-crystal X-ray diffraction. The compound 1 crystallises with triclinic space group P
, a = 9.5923(8) ?, b = 9.8583(8) ?, c = 13.8962(10) ?, α = 89.162(6)°, β = 77.741(7)°, γ = 80.064(7)°, V = 1264.5(2) ?3, Z = 4 and compound 2 crystallises as methanol solvate with monoclinic space group P 21/n, a = 7.5093(9) ?, b = 13.0211(14) ?, c = 16.032(2) ?, β = 92.717(10)°, V = 1565.9(3) ?3, Z = 4. Both crystal structures consist of discrete dimers connected into a three-dimensional network by intermolecular C–H···O
and C–H···X (X = Cl or S) hydrogen bonds and by face-to-face π–π stacking interactions.
Index Abstract The synthesis and structure of two novel N-(benzothiazol-2-yl)benzamides. Irena Ćaleta, Dominik Cinčić, GraceKarminski-Zamola and Branko Kaitner. Hydrogen bonds and
π–π interactions in N-(benzothiazol-2-yl)benzamides N-(benzothiazol-2-yl)benzamides.
相似文献
12.
Chun-Hua Ge Xiao-Yan Zhang Fang Yu Ya-Nan Guo Xiang-Dong Zhang Qi-Tao Liu 《Journal of chemical crystallography》2008,38(7):501-505
Abstract Syntheses and X-ray structural characterizations of two new complexes [Ni(imi)6](pfbz)2 (1) and Cu(imi)2(pfbz)2 (2) (imi = imidazole, pfbz = pentafluorobenzoate) are reported. The first complex crystallizes in the triclinic space group
P-1 with the crystal cell parameters a = 9.180(2) ?, b = 9.742(3) ?, c = 11.466(3) ?, α = 76.947(18)°, β = 80.629(18)°, γ = 78.043(19)°, V = 970.0(4) ?3 and Z = 1. The second complex crystallizes in the triclinic space group P-1 with the crystal cell parameters a = 7.3250(12) ?, b = 7.6685(10) ?, c = 10.888(4) ?, α = 92.80(2)°, β = 101.92(2)°, γ = 115.038(12)°, V = 535.7(2) ?3 and Z = 1. Examination of the structures shows that both complexes form three-dimensional hydrogen bonded networks in which C–H···F
hydrogen bonds play significant roles.
Index Abstract
C–H···F Hydrogen-Bonded Assembly of Ni(II) and Cu(II) Complexes Generate 3D Supramolecular Frameworks
Chun-Hua Ge, Xiao-Yan Zhang, Fang Yu, Ya-Nan Guo, Xiang-Dong Zhang* and Qi-Tao Liu
C–H···F interactions link simple complexes to form intricate three-dimensional supramolecular networks.
相似文献
13.
Chun-nian Xia Wei-xiao Hu Wei Zhou Guo-hong Wang 《Journal of chemical crystallography》2008,38(8):583-586
Abstract The title compound, C16H22O4, synthesized by modified Knoevenagel condensation of protocatechualdehyde with monoheptyl-malonate and recrystallized from
benzene, was confirmed by single-crystal X-ray diffraction (CCDC 272827). The compound crystallizes in triclinic space group
Pī with cell parameters a = 5.296(3) ?, b = 10.711(13) ?, c = 13.870(4) ?, α = 98.84(7)°, β = 90.97(4)°, γ = 96.77(7)° and
Z = 2. The structure is the E isomer and its packing is stabilized by intermolecular O–H···O and C–H···O hydrogen bonds.
Index Abstract The title compound, C16H22O4, synthesized by modified Knoevenagel condensation, was confirmed by single-crystal X-ray diffraction showing its structure
is in E isomer and its packing is stabilized by hydrogen bonds.
相似文献
14.
Pallav D. Patel Tanaji T. Talele Frank R. Fronczek 《Journal of chemical crystallography》2009,39(12):923-926
Abstract
Preparation of oxirane 3 was accomplished in two steps. 1H-1,2,4-triazole was reacted with 2,4-difluoro-α-chloroacetophenone 1 in presence of K2CO3 in refluxing toluene to provide compound 2. Compound 2 was treated with trimethylsulfoxonium iodide (TMSI) in aq. NaOH and toluene to provide oxirane 3. Oxirane 3, previously isolated as an oil, was crystallized from (DCM/MeOH) and characterized by X-ray crystallography: triclinic, space group P − 1, a = 7.3225 (15), b = 7.5833 (15), c = 9.856 (2) Å, α = 91.908 (12), β = 100.824 (11), γ = 103.800 (11)°, V = 520.28 (18) Å3, Z = 2. The molecule has a stepped conformation with nearly parallel triazole and phenyl rings. Lack of classical hydrogen-bond donors leads to packing dominated by weaker interactions, including C–H···N, C–H···F and F···F contacts. 相似文献15.
Synthesis,Characterization and Crystal Structure Determination of a Hepta-coordinated Cadmium(II) Complex with Thiocyanato-bridges 总被引:1,自引:0,他引:1
Dongbin Dang Jide Sun Yan Bai Hui Gao Weili Shang 《Journal of chemical crystallography》2009,39(9):683-687
Abstract A new cadmium(II) complex [(C28H24N6)Cd(SCN)2]2(CH3OH)2 (1) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single crystal X-ray diffraction analysis.
The crystallographic data for compound 1: triclinic P1ˉ, a = 9.630(2) Å, b = 11.123(3) Å, c = 15.396(4) Å, α = 106.93(1)°, β = 91.60(1)°, γ = 99.99(1)°, V = 1,548.5(6) Å3, Z = 1, Dc = 1.512 mg/m3, F(000) = 716, R
1 = 0.0332, wR
2 = 0.0907. The molecule contains a symmetrical dinuclear unit in which two Cd(II) ions are double bridged by two di-μ-1,3-SCN− anoins with a cadmium–cadmium separation of 6.48 Å. Each Cd(II) ion is seven-coordinated with six nitrogen atoms and a sulfur
atom to form a monocapped trigonal prism coordination geometry. In addition, the molecule is further connected by multiform
intermolecular C–H···π, π···π interactions and hydrogen bonds to form a three-dimensional supramolecular structure.
Graphical Abstract A hepta-coordinated Cd(II) complex which exhibits a distorted a monocapped trigonal prism coordination geometry has been achieved
by using bisbidentate Schiff-base ligand and thiocyanate anion.
相似文献
16.
Abstract
Two new complexes [Ni(tren)(pic)]2(ClO4)2·CH3OH (1) and [Co(tren)(dipic)]ClO4·CH3OH (2), (tren is tris(2-aminoethyl)amine, pic is the anion of picolinic acid, dipic is the dianion of 2,6-pyridinedicarboxylic acid) have been synthesized and structurally characterized. X-ray analysis indicates that the two complexes are mononuclear with tren acting as a quadridentate ligand. In complex 1, the nickel(II) ion is further coordinated with picolinate in μ2-N, O bidentate chelating mode. In complex 2, the cobalt(III) ion is coordinated with the pyridine nitrogen and one carboxylic oxygen of 2,6-pyridinedicarboxylate in μ2-N, O chelating form. The metal atoms in both cases have distorted octahedral geometry. Crystal data: [Ni(tren)(pic)]2(ClO4)2·CH3OH (1), Mr = 869.03, monoclinic, C2/c, a = 26.354(5) ?, b = 10.407(2) ?, c = 25.839(5) ?, β = 96.24(3)°, Z = 8, V = 7045(2) ?3, R 1 = 0.0418, wR 2 = 0.1063 [I > 2σ(I)]; [Co(tren)(dipic)]ClO4·CH3OH (2), Mr = 501.77, Triclinic, P-1, a = 8.3667(2) ?, b = 10.4434(2) ?, c = 11.9431(16) ?, α = 73.9590(10)°, β = 88.0240(10)°, γ = 75.5890°, Z = 2, V = 969.97(4) ?3, R 1 = 0.0408, wR 2 = 0.1063 [I > 2σ(I)]. 相似文献17.
Abstract A new ion-pair complex, bis(1-benzyltriphenylphosphinium) bis(1,2,5-thiadiazole-3,4-dithiolato)nickelate(II), [BzTPP]2[Ni(tdas)2](1), has been prepared and characterized by elemental analyses, UV, IR, MS spectrum, molar conductivity and single crystal X-ray
diffraction. The title complex crystallizes in the triclinic space group P-1, a = 9.098(1) Å, b = 9.666(1) Å, c = 29.573(3) Å, α = 83.81(1)°, β = 81.97(1)°, γ = 78.83(1)°, V = 2,517.5(4) Å3, Z = 2. The unit cell contains two [BzTPP]+ and two halves of [Ni(tdas)2]2− anions in which the anion exhibits a quasi-planar structure. The [BzTPP]+ cation adopts a conformation where four phenyl rings are twisted to the C–C–P reference plane. The weak cation–cation C–H···π,
π···π interactions and anion–cation C–H···N hydrogen bonds between the anion and cation play an important role in the stacking
and stabilizing of the title complex.
Graphical Abstract The title new ion-pair complex, bis(1-benzyltriphenylphosphinium) bis(1,2,5-thiadiazole-3,4-dithiolato)nickelate(II), [BzTPP]2[Ni(tdas)2](1), contains two [BzTPP]+ and two halves of [Ni(tdas)2]2− anions in which the weak cation–cation C–H···π, π···π interactions and anion−cation C–H···N hydrogen bonds between the anion
and cation play an important role in the stacking and stabilizing of the title complex.
相似文献
18.
Matloob Ahmad Hamid Latif Siddiqui Saeed Ahmad Graham John Tizzard Masood Parvez 《Journal of chemical crystallography》2010,40(12):1188-1194
Abstract
The crystal structures of four derivatives of pyrazolo[4,3-c][1,2]benzothiazine-2,4-dihydro-3,4-dimethyl-,5,5-dioxide containing benzothiazine dioxide and pyrazolo fused rings that have been synthesized were determined. (C11 H11 N3 O2 S): Mr = 249.29, monoclinic, P21/c, a = 8.3070(3), b = 13.6331(5), c = 10.1661(3) ?, β = 106.924(2)°, V = 1101.45(7) ?3, Z = 4. (C12 H13 N3 O2 S): Mr = 263.31, monoclinic, P21/n, a = 9.729(3), b = 11.224(4), c = 11.436(3) ?, β = 98.85(2)°, V = 1233.9(7) ?3, Z = 4. (C14 H15 N3 O4 S): Mr = 321.35, monoclinic, P21/c, a = 9.2534(3), b = 19.3920(7), c = 7.9489(2) ?, β = 95.323(2)°, V = 1420.21(8) ?3, Z = 4. (C14 H15 N3 O3 S): Mr = 305.35, monoclinic, P21 /c, a = 13.816(7), b = 7.464(3), c = 14.674(8) ?, β = 109.05(3)°, V = 1430.3(12) ?3, Z = 4. The heterocyclic thiazine rings adopt half-chair conformations, and the mean-planes of the phenyl and pyrazolo rings lie between 10.43(11) and 15.93(16)° with respect to each other. In each case, the geometry about thiazine N-atom is trigonal pyramidal and only the first compound containing a donor N-atom shows classical hydrogen bonds. However, non-classical H-bonding of the type C–H···O is observed in all structures. 相似文献19.
Abstract A novel aromatic polycarboxylate polymer, [Zn2(bipy)2(btec)(H2O)2]n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. Compound 1 belongs to the triclinic crystal system, space group P-1; a = 7.7449(6) ?, b = 8.9286(8) ?, c = 10.7422(8) ?, α = 80.95(1)°, β = 70.21(1)°, γ = 78.14(1)°, V = 680.93(10) ?3, Z = 2. The coordination geometry of Zn(II) atom is distorted trigonal bipyramidal with two nitrogen atoms of one 2,2′-bipy
group, two oxygen atoms from two different btec ligands, and one water. The 16-membered rings are alternately arranged forming
an infinite 1-D double-chain structure. A 3-D network was constructed by interlayer C···H–O, O···H–O hydrogen bonds and π–π
stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state.
Graphical Abstract A 1-D double-chain aromatic polycarboxylate polymer, [Zn2(bipy)2(btec)(H2O)2]n (1), has been synthesized and structurally characterized by the single crystal X-ray diffraction. A 3-D network was constructed
by intermolecular C···H–O, O···H–O hydrogen bonds and π–π stacking interactions. Compound 1 exhibits fluorescence at room temperature in the solid state.
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20.
Audra F. Gushwa Yamina Belabassi Jean-Luc Montchamp Anne F. Richards 《Journal of chemical crystallography》2009,39(5):337-347
Abstract The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities,
differences and 31P chemical shifts compared. A series of seven trityl-substituted phosphorus-containing compounds have been characterized by
single crystal X-ray diffraction. Ph3CPPh2, 1, a bulky P(III) compound crystallizes in the triclinic space group , a = 7.5624(6) ?, b = 9.5470(8) ?, c = 16.9722(14) ?, α = 83.4720(10)°, β = 80.541(2)°, γ = 68.1580(10)°, the borane complex of 1, 2, Ph3CPPh2(BH3) crystallizes as monoclinic colorless crystals, P21/c, a = 10.0972(12) ?, b = 9.6955(12) ?, c = 25.197(3) ?, β = 90.258(2)°. The analogous methyl substituted, 3, Ph3CPMe2(BH3) is monoclinic, C2/c, a = 15.628(3) ?, b = 12.770(3) ?, c = 18.406(4) ?, β = 103.968(3)°. Compounds 4–7 are trityl substituted P(V) compounds: Ph3CP(Ph)(O)(OH), 4, crystallizes in the triclinic space group , a = 8.9847(18) ?, b = 9.7443(19) ?, c = 12.786(3) ?, α = 72.045(3)°, β = 72.031(3)°, γ = 78.769(3)°. Esterification of 4 affords TrCP(O)(Ph)OBn 5, space group, P21/c, a = 7.9196(5) ?, b = 31.701(2) ?, c = 19.8062(13) ?, β = 99.7750(10)°. A phosphonate diester was also characterized, Ph3CP(O)(OEt)2, 6, triclinic, , a = 7.9521(17) ?, b = 9.2205(19) ?, c = 14.471(3) ?, α = 85.906(4)°, β = 83.031(4)°, γ = 68.283(4)°. Treatment of the trityl H-phosphinic acid, Ph3CPO2H2, with elemental selenium yields yellow crystals of 7, [Ph3CP(O)(OH)Se]2, P21/c, a = 9.0603(4) ?, b = 22.3652(11) ?, c = 16.9134(7) ?, β = 107.035(2)°. In our efforts to isolate a nickel-phosphine complex, two Ni(II) complexes were crystallographically analyzed,
[Ni(OP(H)Ph2)6]2BF4
−
8 and 9. Complex 8 with an uncoordinated BF4
− ion crystallizes as yellow orthorhombic crystals, Pbca, a = 18.8247(12) ?, b = 18.5518(12) ?, c = 21.0976(14) ?, while crystals of 9 are trigonal, , a = b = 13.1545(12) ?, c = 68.461(9) ?.
Graphical Abstract The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities,
differences and 31P chemical shifts compared.
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