共查询到20条相似文献,搜索用时 31 毫秒
1.
Jaquay Cook Ashleigh Hicks Tyan Frazier David M. Kimari Theodore A. Budzichowski Jeanette A. Krause Bauer Santosh K. Mandal 《Journal of chemical crystallography》2003,33(5-6):481-489
The monodentate dithioformato complexes, fac-(CO)3(dppe)MnSC(S)H (1), fac- (CO)3(dppe)ReSC(S)H (2), fac-(CO)3(dppp)ReSC(S)H (3), and fac-(CO)3 (dppb)ReSC(S)H (4), where dppe is 1,2-bis(diphenylphosphino)ethane, dppp is 1,3-bis(diphenylphosphino)propane, and dppb is 1,4-bis(diphenylphosphino)butane, were synthesized from the treatment of the corresponding hydrides, fac-(CO)3 (P-P)MSC(S)H with CS2. Compounds 1–4 crystallize in the monoclinic crystal system: for 1, space group = P21/c, a = 15.3139(3) Å, b = 9.7297(4) Å, c = 19.0991(6) Å, = 105.928(1), V = 2736.5 Å3, Z = 4; for 2, space group = P21/c, a = 15.6395(8) Å, b = 9.8182(5) Å, c = 19.4153(11) Å, = 106.741(1), V = 2854.9(3) Å3, Z = 4; for 3, space group = P21/n, a = 11.3570(10) Å, b = 19.465(2) Å, c = 15.5702(14) Å, = 104.776(2), V = 3328.3(5) Å3, Z = 4; and for 4, space group = C2/c, a = 32.078(2) Å, b = 10.4741(6) Å, c = 19.0608(9) Å, = 94.315(2), V = 6386.1(6) Å3, Z = 8. 相似文献
2.
Stephanie D. Warner Anne-Marie Lebuis Jean-Pierre Farant Ian S. Butler 《Journal of chemical crystallography》2003,33(3):213-217
In 6-nitrobenzo(a)pyrene, an environmental pollutant, the nitro substituent lies at 69.5(1) to the mean plane of the aromatic moiety. The C–C bond distances range from 1.341(3) to 1.443(3) Å. The crystal is in the monoclinic space group, P21/c, with a = 8.3239(3) Å, b = 8.9530(3) Å, c = 18.0678(5) Å, = 99.264(2) and Z = 4. Molecules are assembled in sheets in the unit cell through stacking and alternating C–H O interactions. 相似文献
3.
Jerry P. Jasinski John M. Jasinski Daniel J. Crosby 《Journal of chemical crystallography》2003,33(5-6):365-374
The crystal structures of the three fluorene related molecules, (I) 2-(9,9-dipropylfluorene-2-yl)-9,9-dipropylfluorene, [Exalite 384, C38H42], (II) 2-(1,1-dimethylpropyl)-7-{4-[(1,1-dimethylpropyl)-9,9-diethylfluoren-2-yl] phenyl}-9,9-diethylfluorene, [Exalite 404, C50 H58], and (III) 2-(4-ethylphenyl)-7-[7-(ethylphenyl)-9,9-dipropylfluoren-2-yl]-9,9-dipropylfluorene, [Exalite 416, C54H58], have been determined. Structural details reveal a novel new bonding arrangement at the C2 atoms of symmetry-related fluorene moieties in all three molecules producing a linear type array with an inversion center connecting adjacent asymmetric units within each molecule. Exalite 384 is monoclinic, space group P21/c with a = 9.002(2) Å, b = 16.275(4) Å, c = 10.525(1) Å, = 103.05(1), and V = 1502.1(5) Å3 with Z = 4, for d
calc = 1.103 g/cm3. Exalite 404 is triclinic, space group P1 with a = 10.383(1) Å, b = 13.404(2) Å, c = 7.7007(9) Å, = 105.296(9), = 104.23(1), = 73.707(9), and V = 974.9(2) Å3 with Z = 2, for d
calc = 1.141. Exalite 416 is monoclinic, space group P21/c with a = 15.99(10) Å, b = 11.178(8) Å, c = 23.766(4) Å, = 104.21(4), and V = 4117(4) Å3 with Z = 4, for d
calc = 1.141 g/cm3. 相似文献
4.
Ping-Yu Bu Lei Z. Zhang Li-Cun Li Peng Cheng Shi-Ping Yan Zong-Hui Jiang Dai-Zheng Liao 《Journal of chemical crystallography》2003,33(4):257-262
A terephthalato-bridged copper(II) complex [Cu2(tpt)(bpy)2(H2O)4][Cu2(tpt)3(bpy)2 (H2O)2] (1) (tpt = terephthalate, bpy =; 2,2'-bipyridine) was synthesized by the reaction of Cu(ClO4)2 6H2O and terephthalic acid in the presence of 2,2'-bipyridine in H2O solution. Crystal structure of 1 was determined by X-ray diffraction analysis in the triclinic space group P
, with a = 10.7327(10) Å, b = 11.1658(11) Å, c = 17.3768(16) Å, = 108.063(2), = 91.064(2), = 116.721(2), V = 1737.5(3) Å3, and Z = 2. Both the anion and the countercation in 1 are copper(II) complexes linked by terephthalate bridges in the bis(monodentate) (syn–anti) mode. The anion and the countercation are also linked by two hydrogen bonds between coordinating water molecules and terephthalate ligand. 相似文献
5.
Lawrence C. Thompson Kyle S. Knight William T. Pennington 《Journal of chemical crystallography》2003,33(5-6):403-407
A triphenyl analog of taddol, 4-R,5-R-[5-(hydroxy-diphenyl-methyl)-2,2-dimethyl-[1,3]dioxolan-4-yl]-phenyl-methanone, has been synthesized and structurally characterized. This molecule could act as a chiral ligand building block in the creation of tuned taddol analogs. Structural analysis of the title compound reveals that the hydroxyl group is involved in an intramolecular hydrogen bond and does not take part in any intermolecular interaction. Crystal packing is influenced by C–H O hydrogen bonding and phenyl phenyl interactions. Crystal data: Triclinic, P1 (No. 1), a = 5.9343(4) Å, b = 8.2367(17) Å, c = 10.987(2) Å, = 88.290(6), = 75.442(4), = 80.655(6), V = 512.86(15) Å3, Z = 1, D
calc = 1.258 mg/m3. Final residual values were R
1 = 0.0407 for 3022 observed data (I > 2s(I) ) and wR
2 = 0.0941 for all 3524 unique data. 相似文献
6.
Zahida Shirin Brian S. Hammes Chris R. Warthen Carl J. Carrano 《Journal of chemical crystallography》2003,33(5-6):431-436
Reaction of the Zn, Cd, or Co nitrate salts with the deprotonated ligand (2-hydroxy-3-t-butyl-methylphenyl)bis(3,5-dimethylpyrazolyl)methane (L1O–) in methanol produced the following complexes: [(L1OH)Zn(NO3)2] in two isomorphs, a = 40.983(8) Å, b = 9.571(2) Å, c = 15.667(8) Å, = 90, = 106.38(1), = 90, C2/c, and a = 13.027(3) Å, b = 14.781(4) Å, c = 16.107(3) Å, = 90, = 105.30(1), = 90, P21/n; [(L1OH)Cd(pz)(NO3)2] a = 14.7476(2) Å, b = 13.5411(2) Å, c = 16.7223(2) Å, = 90, = 110.3840(10), = 90, P21/c; and [(L1O)Co(pz)(NO3)] a = 11.4240(2) Å, b = 13.4498(2) Å, c = 13.8056(2) Å, = 105.2080(10), = 105.8130(10), = 112.7470(10), P
. The Zn adopts a pseudotetrahedral four-coordinate geometry where the potentially tridentate ligand is actually bidentate with a protonated and uncoordinated phenoxy arm. The Co complex is pseudooctahedral six-coordinate where the phenoxy arm is deprotonated and coordinated. Finally the Cd complex is seven-coordinate but the metal is not coordinated through the phenoxy group that is again protonated. 相似文献
7.
Simon G. Bott Kaiyuan Yang Michael G. Richmond 《Journal of chemical crystallography》2003,33(7):585-588
The structure of (5S)-3,4-dichloro-5-menthoxy-2(5H)-furanone is reported. The title compound crystallizes in the monoclinic space group P21: a = 6.650(2) Å, b = 8.038(3) Å, c = 14.858(8) Å, = 97.01(3), V = 788.3(6) Å3, Z = 2, R = 0.0718, R
w = 0.0795 for 735 observed reflections with I > 3 (I), and the absolute configuration at C-5 of the furanone ring is shown to be (S). 相似文献
8.
A novel heteronuclear complex, [NdZn2L6(NO 3)(phen)2] (HL = -methylacrylic acid, phen = 1,10-phenanthroline), was synthesized and characterized by elemental analysis, infrared absorption spectra (IR) and its molecular structure was also determined by X-ray structure analysis. The title complex contains a discrete trinuclear ZnNdZn molecule bridged by carboxylate groups between Zn and Nd ions and crystallizes in space group P¯1 with the cell dimensions: a = 13.601(3) Å, b = 16.859(2) Å, c = 12.575(2) Å, = 110.09(1), = 112.21(1), = 81.10(2). 相似文献
9.
Deborah C. Bebout James F. Bush II Elizabeth M. Shumann Julie A. Viehweg Margaret E. Kastner Damon A. Parrish Steven M. Baldwin 《Journal of chemical crystallography》2003,33(5-6):457-463
The dimeric mercurous ion has been encapsulated by a pair of the tetradentate tripodal nitrogen ligands tris[(2-(6-methylpyridyl))methyl]amine (TLA). The complex [Hg2(TLA)2](ClO4)2 (1) was isolated directly from an acetonitrile solution of Hg(ClO4)2 3H2O and TLA. Complex 1 crystallizes in the triclinic space group
with a = 10.537(2) Å, b = 10.751(2) Å, c = 10.907(2) Å, = 75.20(3), = 73.73(3), = 75.73(3), and Z = 1. The cation is located an inversion center. The Hg–Hg and Hg–Namine bond distances are 2.5469(8) and 2.297(6) Å, respectively, and the average Hg–Npyridyl bond length is 2.75(7) Å. Complex 1 was stable indefinitely in acetonitrile-d
3 solution, permitting detection of 13 and 22 Hz heteronuclear couplings between the Hg(I) ions and the methylene protons of the ligand. Comparisons with the structures and spectroscopic properties of related mercuric and mercurous complexes are made. 相似文献
10.
Douglas X. West Jerry P. Jasinski John M. Jasinski Ray J. Butcher 《Journal of chemical crystallography》1999,29(10):1089-1095
Structures of two binuclear copper(II) complexes with sulfato bridges and tridentate 2-acetylpyridine 3-azacyclothiosemicarbazone ligands have been solved. The complex-sulfato-bis{(2-acetylpyridine 3-hexamethyleneiminyl-thiosemicarbazonato)copper(II)} N,N-dimethylformamide, [Cu(Achexim)]2SO4·DMF, has the following structural properties: triclinic, P1¯(#2), a = 12.314(4), b = 15.885(4), c = 10.959(4) Å, = 103.25(2), = 103.60(2), = 109.94(2)°, V = 1843(2) Å3, and Z = 2; for -sulfato-bis{(2-acetylpyridine 3-piperidylthiosemicarbazonato)copper(II)}chloroform, [Cu(Acpip)]2SO4·CHCl3: triclinic, P1¯(#2), a = 11.657(1), b = 17.101(2), c = 10.338(1) Å, = 98.51(1), = 109.294(7), = 107.016(9)°, V = 1790.3(4) Å3, and Z = 2. The size of the azacyclo ring significantly affects the stereochemistry of these binuclear complexes. 相似文献
11.
Andrew S. Albrecht Christopher P. Landee Mark M. Turnbull 《Journal of chemical crystallography》2003,33(4):269-276
Reaction of 2-amino-5-methylpyridine with zinc chloride and HCl in aqueous solution yields bis(2-amino-5-methylpyridinium) tetrachlorozincate. The complex crystallizes in the monoclinic space group P21/c, with minimal tetrahedral distortion of the ZnCl4
2– ion at both 298 and 150 K; at 298 K, a = 8.090(2) Å, b = 14.795(6) Å, c = 15.850(4) Å, = 101.93 (2); at 150 K, a = 8.0986(2) Å, b = 14.7190(5) Å, c = 15.7684(7) Å, = 102.862(2). The anisotropic cell contraction results in significant changes in nonbonding Cl Cl contacts. 相似文献
12.
Wang Qing-Min Liu Gang Shao Rui-Lian Huang Run-Qiu 《Journal of chemical crystallography》2004,34(1):31-37
The title compound 3,5-di(2-propenyl)-6-phenyl-1,3,5-triazine-2,4-dione has been synthesized by the reaction of 6-phenyl-1,3,5-triazine-2,4-dione with allyl bromide. Its structure was determined by X-ray single crystal diffraction. The crystal belongs to orthorhombic, space group Pbca with the following crystallographic parameters: a = 16.282(4) Å, b = 8.888(2) Å, c = 19.281(5) Å, = 90°, = 90°, = 90°, = 0.088 mm–1, V = 2790.1(13) Å3, z = 8, Dx = 1.282 mg/m3, F(000) = 1136, T = 293(2) K, 2.11° 25.02°, the final R factor: R
1 = 0.0430, wR2 = 0.0981. The X-ray results demonstrate that the reaction of 6-phenyl-1,3,5-triazine-2,4-dione with allyl bromide in the presence of N,N-dimethylformamide and potassium carbonate yields the N-alkylated product. The title compound 2-dimethylamino-4-ethoxycarbonylmethoxy-6-phenyl-1,3,5-triazine has been synthesized by a new reaction, in which the solvent N,N-dimethylformamide involves. Its structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic, space group P-1 with the following crystallographic parameters: a = 7.977(2) Å, b = 10.394(3) Å, c = 10.837(3) Å, = 111.774(5)°, = 104.050(5)°, = 99.446(5)°, = 0.093 mm–1, V = 776.6(4) Å3, z = 2, Dx = 1.293 mg/m3, F(000) = 320, T = 293(2) K, 2.14° 25.03°, the final R factor: R
1 = 0.0582, wR
2 = 0.1399. The distance of N(4)
C(2) (1.339 Å) is much shorter than the length of normal C
N (1.47 Å) and very close to that of C-N (1.33 Å), which is indicative of the significant double bond character. 相似文献
13.
Andrea M. Goforth Mark D. Smith Hans-Conrad zur Loye 《Journal of chemical crystallography》2003,33(4):303-306
The two-dimensional coordination polymer [Cu2
i
2(pyz)]n (where pyz = pyrazine) has been synthesized hydrothermally and structurally characterized by single crystal X-ray diffraction analysis. [Cu2
i
2(pyz)]n crystallizes in the space group P
with a = 4.1759(4) Å, b = 7.1281(7) Å, c = 8.1279(8) Å, = 109.607(2), = 101.769(2), = 96.676(2), and Z = 1. The sheet-like polymer is characterized by infinite stair step [Cu2
i
2]n double chains connected in two dimensions through bridging pyrazine ligands. The coordination environment about each copper is approximately tetrahedral having three Cu–I bonds and a single Cu–N bond. 相似文献
14.
The crystal structure of [SnBu2(TNEE)2], (HTNEE=5-ethyl ester of 2-mercaptopyridine-5-carboxylic acid) has been determined by X-ray single crystal diffraction study. The crystal is triclinic, space groupP,a=10.042(1),b=18.421(2),c=7.979(1) Å, =98.7(1), =107.3(1), =87.7(1)o,V=1393(1) Å3, and Z=2 The tin center is coordinated to two butyl groups and to the nitrogen and the sulfur atoms of two ligand molecules in a very distorted trapezoidal bipyramid. 相似文献
15.
S. Shanmuga Sundara Raj M. N. Ponnuswamy G. Shanmugam M. Kandaswamy 《Journal of chemical crystallography》1993,23(7):607-610
The crystal and molecular structure of the title compound, C20H32N2O3, has been determined from X-ray diffraction data using CuK radiation (=1.5418 Å). The compound crystallizes in triclinic space groupP1¯ with a=8.828(1),b=18.680(1),c=6.272(2)Å, =93.42(1), =0.24(2), =77.93(1)°,V=1009.4(2)Å3, andZ=2. The structure was solved by direct methods and the full-matrix least-squares refinement leads the finalR-factor to 0.065 for 3481 observed reflections withI3(I). The phenyl ring is planar and the morpholino rings assume perfect chair conformation. The molecules are held together by van der Waals forces.DCB Contribution No. 810. 相似文献
16.
Jeffrey C. Bryan Benjamin P. Hay Richard A. Sachleben Cassandra T. Eagle Cungen Zhang Peter V. Bonnesen 《Journal of chemical crystallography》2003,33(5-6):349-355
The podand, bis(2-methoxyphenoxy)m-xylene (1), was designed and synthesized as a potential host for the cesium ion. Its structure was determined by single crystal X-ray diffraction. It crystallizes in P21/c with cell dimensions: a = 8.5723(7) Å, b = 8.3931(14) Å, c = 25.2879(26) Å, = 96.224(9), and V = 1808.7(4) Å3. A crown derivative, tribenzo-21-crown-6 (2), was also prepared and structurally characterized. It also crystallizes in P21/c with cell dimensions: a = 15.5825(13) Å, b = 15.8648(16) Å, c = 8.8266(7) Å, = 95.247(6), and V = 2172.9(3) Å3. The structures exhibit hydrogen bonding, and are evaluated in terms of complementarity and preorganization for cesium binding. 相似文献
17.
De-Zhong Niu Lai-Long Mu Shou-Zheng Yu Jiu-Tong Chen 《Journal of chemical crystallography》2003,33(1):27-31
The synthesis as well as crystal and molecular structure of [Bi(C5H4NOS)3] are reported. The complex crystallizes in the monoclinic system, space group P21/n with lattice parameters a = 9.6521(3) Å, b = 10.0659(4) Å, c = 18.4484(7) Å, = 102.13(6)°, and D
calc = 2.227 Mg · m–3 for Z = 4. It is clear from the packing diagram that the title compound is a dimer via the secondary coordination. Surrounding Bi atom, three five-membered ring planes (Bi,O,N,C,S) make a dihedral angle of 55.91, 54.72, and 26.13° respectively. The whole crystal presents a three-dimensional network structure as each molecule produces four weak C–H O hydrogen bonds and a weak C–H S hydrogen bond. 相似文献
18.
Synthesis and X-ray structural investigations have been carried out for the two title compounds C14H10N2O (3a) and C22H26N2O (3b). Compound 3a crystallizes in the monoclinic space group P21/c, with a = 3.843(1) Å, b = 24.618(5) Å, c = 11.318(2) Å, = 92.61(3), V = 1069.7(4) Å,3 and Z = 4. Compound 3b crystallizes in the triclinic space group P-1, with a = 9.004(2) Å, b = 9.447(2) Å, c = 11.713(2) Å, = 76.70(3), = 83.12(3), = 82.16(3), V = 956.5(3) Å,3 and Z = 2. Both stilbazole derivatives have Z-geometry about the ethylene bridge which links the heterocyclic and aromatic rings. The molecular skeleton of 3a is slightly non-planar: the dihedral angles between the acrylonitrile linkage and the pyridine ring, and between this linkage and the p-hydroxyphenyl ring are 7.2(2) and 4.1(2), respectively. The molecular skeleton of 3b is less planar: the values of similar dihedral angles are 17.0(2) and 20.8(2), respectively. In the crystal of 3a, the molecules are packed in stacks along the a axis with head-to-head orientation. Intermolecular hydrogen bonds O=H s N and C=H s N link molecules into sheets parallel to (100) plane. In the crystals of 3b, the molecules have a head-to-tail orientation and intermolecular hydrogen bonds O=H s N link the molecules into infinite chains along [01-1] direction. 相似文献
19.
A novel oxovanadium(IV) complex with tridentate schiff base and bidentate phenanthroline ligands, VO(o-van)(phen) 2H2O[o-van-gly: o-vanillin-glycine; phen: phenanthroline], was synthesized and characterized by elemental analysis, IR and UV-vis spectra. The crystal structure was determined by X-ray single crystal diffraction analysis. The crystal of title complex (C22H21N3O7V, Mw = 490.36) belongs to triclinic, space group P-1 with the following crystallographic parameters: a = 9.247(3) Å, b = 10.125(4) Å, c = 13.100(5) Å, = 106.343(6), = 96.042(7), = 101.726(7), V = 1135.0(7) Å3, Z = 2, Dc = 1.435 Mg m–3, (MoK = 0.485 mm–1, F(000) = 506, and final R1 = 0.0779, wR2 = 0.1598 for observed reflections 1606 (I > 2(I)). V(IV) is six-coordinate with three oxygen atoms and three nitrogen atoms in a distorted octahedral geometry. The complex forms a 3-D network via – stacking and hydrogen bonds. 相似文献
20.
Martijn J.J. Mulder Huub Kooijman Anthony L. Spek Jaap. G. Haasnoot Jan Reedijk 《Journal of chemical crystallography》2002,32(9):347-351
The crystal structure of the title compound, tetrabutylammonium bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate(III), [N(C4H9)4][Ni(C3S5)2], is the fourth known phase of this polymorphous compound. It is monoclinic space group P21/c, with a = 20.040(2) Å, b = 13.1151(17) Å, c = 12.1093(15) Å, = 105.456(15)°, and V = 3067.5(6) Å3 with Z = 4, for D
calc = 1.503 g cm–3. The [Ni(dmit)2] anion packing arrangement consists of arrays of side-on touching anions and these arrays are connected via head-to-tail close S S contacts. 相似文献