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1.
V. Venkatachalam K. Ramalingam Thomas C. W. Mak Bao-Sheng Luo 《Journal of chemical crystallography》1996,26(7):467-470
The title compound was synthesized by the interaction of arsenic(III)chloride with freshly prepared N-methylaminoethanoldithiocarbamic acid in methanol. The compound crystallized in the triclinic system, space groupP with two molecules per unit cell, the dimensions area=6.509(10)Å,b=14.077(3)Å,c=14.195(3)Å, =64.16(2)o, =84.67(2)o and =84.00(2)o. The molecule is monomeric with three short (mean 2.320(3)Å) and three long (mean 2.927(2)Å) As-S bonds. Asymmetry in the As-S bonds is due to the presence of stereochemically active lone pair on arsenic and the coordination polyhedron deviates from the usual D3 symmetry to C3 symmetry. Disorder exists in one of the dithiocarbamate ligands probably due to the O...O interaction arising from the water molecule. The anisobidenticity of the As-S bond distances is as a consequence of stereochemical requirement of the ligand and the lone pair of electrons on arsenic. 相似文献
2.
Jason A. Kautz Donald F. Mullica J. Matt Farmer 《Journal of chemical crystallography》1999,29(6):729-733
The structural analysis of [(n-C4H9)4N]3[Y(NCS)6] (I) using single-crystal diffraction data and full-matrix least squares refinement has been carried out. The hexaisothiocyanate complex crystallizes in the centrosymmetric triclinic space group P
(No. 2) with unit cell constants of a = 12.431(1), b = 12.866(1), c = 22.750(2) Å, = 90.78(1), = 92.05(1), = 96.67(1)°, and Z = 2. The molecular unit consists of three separate cationic tetra-n-butylammonium groups and an independent hexakisisothiocyanatoyttrate anionic group in which the six thiocyanate ligands are octahedrally coordinated through the N atom to the Y central ion. Selected bond distances and angles are presented as well as the synthesis and peripheral studies of (I). 相似文献
3.
John Emsley Muhammad Arif Paul A. Bates Michael B. Hursthouse 《Journal of chemical crystallography》1987,17(5):605-613
C12H14CuF2N2O3,M=335.797, monoclinic, space groupP21/n,a=6.985(2),b=17.406(2),c=10.581(2) Å,=92.41(2)°,V=1285(1) Å3,D
c
=1.736 g cm–3,Z=4,F(000)=684,(CuK)=27.0 cm–1, =1.5418 Å,T=20°C, crystal dimensions=0.75×0.45×0.30 mm. The structure of the title compound shows it to be [Cu(phen)F2(H2O)]·2H2O with pentacoordinate-square pyramidal Cu(II), short Cu-F bonds [1.890(4) and 1.891(4) Å], and short FH-O hydrogen bonds (ca. 2.68 Å) between the complex and lattice water molecule. 相似文献
4.
Bijan Etemadi Abdol Abadi Rex A. Palmer Brian W. Fitzsimmons 《Journal of chemical crystallography》1988,18(1):35-53
The crystal structure of bis (NN-di(n-propyl)dithiocarbamato iron(III) iodide, FeIII(S2CN6H14)2I, has been determined by the heavy-atom method and refined toR=0.055 for 3487 reflections withI(hkl)>3I(hkl). The crystals are triclinic,C¯1,Z=8,a=27.644(6),b=19.186(4),c=8.694(2) Å,=87.79(1),=88.72(1), =101.87(2)°. The I-Fe bond lengths are different in the two moleculesA andB in the asymmetric unit, having values of 2.642 Å (2.655) and 2.612 Å (2.634) respectively (libration-corrected values given in parentheses). The measured effective magnetic moment
eff3.89 BM, independent of temperature (93-353K), suggests a spinS of 3/2 with three unpaired electrons for FeIII. 相似文献
5.
The structure of triphenylphosphine — (1 — (di(trifluoromethyl) — hydroxymethyl) — cyclopentadienyl) — (1,2 — di(carboxymethyl)ethylene — 1 — yl) — ruthenium (0) has been studied by single-crystal X-ray diffraction techniques. This compound, [C5 H4(CF3)2 COH] Ru(PPh3)C2(CO2Me)2H, crystallizes in the triclinic space groupP¯1 witha =10.131,b= 15.107,c= 10.798 Å, = 102.14, = 107.04, = 89.64° andZ = 2. The structure was refined by block-diagonal least-squares methods to a finalR value of 0.042, including hydrogen atoms. The compound contains a dicarboxymethylethylene ligand coordinated to ruthenium both through a ketonic oxygen and through a metal--carbon -bond. An intramolecular hydrogen bond is observed. Details of the structure are reported, and the structures of several Ru(0) complexes are compared. 相似文献
6.
Jeroen van Westrenen A. Dean Sherry Won Dae Kim Anne E. Vivian Duane C. Hrncir 《Journal of chemical crystallography》1993,23(11):885-890
C5H10N2O3S,1, monoclinicC2/c,a=17.545(5),b=6.822(8),c=13.928(2),=108.36(7),Z=8, MoK, =0.7107 Å,=3.56cm–1,R=0.061,R
w
=0.099. C8H16N3O6S2Na·2H2O,2, orthorhombicPna21,a=17.964(8),b=10.157(1),c=8.263(4),Z=4, MoK, =0.7107 Å,=4.07 cm–1,R=0.040,R
w
=0.043. C10H20N4O6S2·2H2O,3, monoclinicP21/n,a=9.142(9),b=13.576(7),c=14.028(8),=94.096(8),Z=4, MoK, =0.7107 Å,=3.37 cm–1,R=0.063,R
w
=0.074. Compounds1, 2, and3 were prepared from the pH-dependent sulfomethylation of the di- and polyazamacrocycles. 相似文献
7.
Joan Ribas Montserrat Monfort Carmen Diaz Manuel Font-Altaba Xavier Solans 《Journal of chemical crystallography》1987,17(3):303-312
The title compound is orthorhombic,M
r
=590.2,P212121 (No. 19),a=9.865(2),b=9.924(2),c=31.202(7) Å,V=3055(2) Å3,Z=4,D
x
=1.283 g cm–3, (MoK
);F(000)=1256; (MoK
)=6.76 cm–1, finalR=0.052 for 1441 reflections I2.5(I). The nitrite group is chelated via the two oxygen atoms; the two six-membered rings resulting from the coordination of the 1,3-propanediamine ligands to the nickel(II) atom are in the chair conformation. The Ni-N and Ni-O distances average 2.07(1) and 2.14(2) Å respectively. The two Ni-O distances are nearly equivalent. 相似文献
8.
1,4-diphenylbutadiyne, C16H10, crystallizes in monoclinic space group P21/n witha=6.6152(6),b=6.0768(7),c=14.634(1) Å, =100.981(8)0,V=577.5(2) Å3,Z=2. The structure was refined toR=0.077 andR
w=0.069 for 1007 observed reflections with CuK radiation. The molecule lies on an inversion center. Our determination represents and increase in precision of a factor of approximately three over the original determination. The 21 cobalt complex, C16H10[Co2(CO)6]2, also crystallizes in monoclinic space group P21/n witha=8.9568(12),b=17.7057(10),c=18.5671(12) Å, =90.606(12)o,V=2944.3(5) Å3,Z=4. The structure was refined toR=0.032 andR
w=0.031 for 4312 observed reflections. The diphenylbutadiyne triple bonds elongate to 1.346(3) Å and the angles at the diyne C atoms decrease to 134.1(3)–144.9(3)o upon complexation. The Co-Co distance is 2.4580(4)Å. Our data represent an increase in precision by a factor of 2–3 over the original determination. 相似文献
9.
J. M. M. Smits P. T. Beurskens R. Plate H. C. J. Ottenheijm 《Journal of chemical crystallography》1986,16(6):957-966
The structure of the title compound, C18H20N2O5, was determined by X-rays atT=290 K.M
r
=344.366, monoclinic, space groupP21/c,a=13.7850(8),b=8.8951(7),c=15.1603(11) Å, =111.410(6)°,V
c
=1730.7 Å3,Z=4,D
x
=1.322 Mgm–3. Cu K radiation (graphite crystal monochromator, =1.54178 Å),(Cu K)=7.69 cm–1. Final conventionalR-factor=0.057,R
w
=0.076 for 2160 observed reflections and 271 variables. The structure was solved usingMultan. 相似文献
10.
Slaheddine Chaabouni Jean Michel Savariault Abdelhamid Ben Salah 《Journal of chemical crystallography》2004,34(3):223-227
The salt di(N-benzyl piperidinium) pentachloroantimonate(III) dihydrate crystallizes in the orthorhombic system with space group Cmc21, the unit cell dimensions are: a = 29.383(1), b = 10.509(2), c = 9.941(1) Å, with Z = 8. The structure shows a layer arrangement perpendicular to the a axis: planes of SbCl6 octahedra alternate with planes of [C12H17N]+ cations. The SbCl6 octahedra are connected through a O(W)–HCl hydrogen bonds and a chlorine bridge, so that infinite unidimensional chains of composition [SbCl5(H2O)2]2n–
n are formed in the structure along the c direction. These chains are connected to [C12H17N]+ entities by N–HCl and N–HO(W) hydrogen bonds, forming a three-dimensional network. It was found that lengths of Sb–Cl bonds may differ from each other. The differences shown as a distortion of the SbCl6 octahedra were attributed to the Sb(III) lone electron pair stereoactivity. 相似文献
11.
Yu-Ying Hsieh Yeong-Horng Sheu I-Chih Liu Chu-Chieh Lin Jyh-Horung Chen Shin-Shin Wang Hann-Jenn Lin 《Journal of chemical crystallography》1996,26(3):203-207
The title compound, Ga(tpp)(OAc), crystallizes in the space group P21/n witha=10.628(2),b=16.176(2),c=20.750(2), Å, =92.64(2)°, andZ=4. The gallium atom has a squarepyramidal coordination geometry formed by the four nitrogen atoms of the porphyrinato group (Np) and the acetate ion. The geometry around the gallium center of the Ga(tpp)(OAc) molecule has Ga–O(1)=1.874(4) Å and average Ga–Np(porphyrin nitrogen)=2.056(4) Å. The acetate group is unidentately coordinated to the gallium (III) atom. Ga-71 NMR spectroscopy provides a complementary method for investigation of the acetate ligand. Combining the calculated value of c, 29.0 ps, with the measured Ga-71 quadrupolar relaxation time, T1Q=11.1 s, the quadrupole coupling constant of Ga-71 is 28.1 MHz. This further supports that Ga is covalently coordinated to the acetate and tpp in Ga(tpp)(OAc). The methyl and carbonyl carbons of the acetate group are separately located at 20.4 and 168.8 ppm at 24°C for the Ga(tpp)(OAc). 相似文献
12.
S. Shanmuga Sundara Raj M. N. Ponnuswamy G. Shanmugam M. Kandaswamy 《Journal of chemical crystallography》1994,24(1):83-87
MMP: C17H26N2O3,M
r
=306.40, monoclinic, space groupP21/c,a=10.927(2),b=10.777(2),c=14.197(2) , =94.04(2)°,V=1667.7(5) 3,D
cal=1.22 Mgm–3,Z=4,F(000)=664, =5.93 cm–1,T=293K. FinalR=0.049 andwR=0.063 for 2724 observed reflections. MBrP; C16H23N2O3Br,M
r
=371.27, monoclinic, space groupP21/c,a=10.955(1),b=10.785(1),c=14.213(1) , =94.54(2)°,V=1674.0(4) 3,D
cal=1.48 Mgm–3,Z=4,F(000)=768, =32.35 cm–1,T=293K. FinalR=0.055 andwR=0.069 for 2886 observed reflections. MMP and MBrP are isostructural and in both the molecules the morpholino rings assume a chair conformation.DCB Contribution No. 824. 相似文献
13.
Thomas S. Janik Lynn M. Krajkowski Melvyn Rowen Churchill 《Journal of chemical crystallography》1995,25(11):751-754
The title compound crystallizes in the centrosymmetric triclinic space group
(No. 2) witha=10.818(1)Å,b=10.876(1)Å,c=11.072(2)Å, =98.74(1)°, =98.83(1)°, =96.61(1)°,V=125906(3)Å3 andZ=2. Interatomic distances include Fe–P=2.243(2)Å, Fe–CO=1.771(6)–1.781(5)Å, Fe–C(C5H5)=2.074(6)–2.103(5)Å and P–F=1.511(6)–1.571(4)Å. 相似文献
14.
Sanjeev Bhargava Rakesh Bohra R. C. Mehrotra 《Journal of chemical crystallography》1991,21(3):281-285
The title compound has been synthesized by the reaction of CrCl36H2O with K{S2COCH(CH3)2} in a 13 molar ratio in an aqueous medium. It has been characterized by elemental analysis and IR spectral studies. Crystals of Cr{S2COCH(CH3)2}3 are monoclinic, space group P21/n witha=10.002(2),b=10.973(1),c=18.961(6) Å,=91.78(2)°,V=2079.9 Å3,Z=4,D
calc=1.46 g cm–3, monochromatic radiation (Mo-K), =0.71069 Å,=11.2 cm–1,F(0 0 0)=948,T=295K, finalR=0.0320 for 2641 reflections. The environment of the chromium atom is based on an octahedral geometry having six sulfur donor atoms from three symmetrically chelated ligands with average distances: Cr-S=2.396(9) Å, C-S=1.690(3) Å and C-O=1.315(3) Å. The bond distance between oxygen atom and the carbon atom of the isopropyl group (O-Cav=1.478(4) Å) suggests that the form –S
2
(–)
C=O(+)CH(CH3)2 contributes significantly to the structure of the isopropyl group. 相似文献
15.
The crystal structure of metalaxyl (C15H21NO4) was determined by three-dimensional X-ray analysis from diffractometer data. The crystals are monoclinic,P21/c,a=7.851(3) Å,b=13.119(10) Å,c=15.107(7) Å,=101.71(6)°,Z=4,D
x=1.218 g cm–3, (MoKa)=0.095 mm–1. FinalR=0.079 for 1203 observed reflections. The dimethylphenyl ring is almost perpendicular to the amidic plane of the molecule. 相似文献
16.
A. M. Atria R. Baggio M. T. Garland O. González J. Manzur O. Peña E. Spodine 《Journal of chemical crystallography》1993,23(12):943-947
The synthesis, structure and magnetic properties of [Cu(diMe-bipy)Br2] are reported (diMe-bipy=4,4-dimethyl 2,2-bipyridine). The complex has a polymeric structure composed of [Cu(diMebipy)Br2] subunits linked via bridging bromine atoms. Each copper atom is hexacoordinated in a distorted octahedral coordination environment. Crystallographic data: monoclinic, space groupC2/c,Z=4, unit cell of dimensionsa=18.312(7),b=9.818(2),c=7.486(2)Å,=107.750(0)° at 293 K. The best fit of the magnetic susceptibility data by the uniform Heisenberg chain model forS=1/2 ions yields values for the exchange coupling constant of –0.46 cm–1. The magnetic susceptibility of the dimeric [Cu(diMe-bipy)Cl2]2·0.5H2O exhibits a maximum near 12 K that is indicative of an antiferromagnetic interaction between the two metal centers. The best fit of the experimental data by the Bleaney-Bowers equation was obtained withg=1.95 andJ=–6.99 cm–1. 相似文献
17.
Franz Effenberger Ingrid Barthelmess Norbert Rösch 《Journal of chemical crystallography》1995,25(8):493-498
The red colored and poorly soluble 1,6-bis(o-hydroxyanilino)-1,5-hexadiene-3,4-dione (3f) forms stable adducts5 and7 of exact stoichiometric ratios withN,N-dimethyl carboxamides4 and ureas6. The adducts are yellow colored and easily soluble in organic solvents. The crystal structure of3f (monoclinic space groupP2
1/c witha=7.903(2),b=10.941(2),c=8.976(3) Å, =90.13(2)°) indicates planarity with extensive delocalization of the -electrons. The poor solubility is referred to the formation of strong intermolecular hydrogen bonds (H(O)...O3 andH(O)...O3=1.79 Å). The crystal structure of the 12 DMF adduct5a (monoclinic space groupP2
1/c witha=6.068(1),b=19.668(2),c=10.645(1) Å, =107.791(8)°) shows a less pronounced delocalization of the -electrons which might be the explanation for the color change from red to yellow. In5a the intermolecular hydrogen bonds of3f are interrupted by forming new hydrogen bonds from the hydroxyl group to the carbonyl group of DMF (H(O)...O(L) andH(O)...O(L)=1.86 Å), whereby the solubility is markedly changed. The thermal stability of the addition products5 and7 was determined by thermogravimetry. 相似文献
18.
Francesco Bigoli Maurizio Lanfranchi Maria Angela Pellinghelli 《Journal of chemical crystallography》1989,19(2):357-367
Crystal structure analyses of urazine and of its adduct with CuCl2 show that this ligand can exchange interactions of stacking that cannot be defined as simple - interactions. The copper atoms are octahedrally coordinated by two oxygen atoms and two aminic nitrogen from chelating uraxines and two chlorine atoms. The crystals of urazine are monoclinicP21
c:a=6.741(1),b=5.815(1),c=11.141(2) Å,/gb=92.13(1)°,V
c=436.4(1) Å3,Z=4,R=0.0402 for 714 independent observed reflections; the crystals of [CuCl2(urazine)2] are triclinicP¯1:a=5.236(1),b=6.662(1),c=8.411(1) Å,=93.00(1),=104.87(1), =105.69(1)°,V
c=270.66(8) Å3,Z=1,R=0.0380 for 875 independent observed reflections. 相似文献
19.
The title compound (C18H26N6Cl2) crystallizes in monoclinic space group P21/c with a = 14.867(4) Å}, b = 7.758(2) Å}, c = 9.671(3) Å}, = 108.78(1), V = 1056.0(5) Å}3, Z = 2, Dcal = 1.250 Mg/m3 at T = 293 K. The structure was solved by direct methods and refined by full-matrix least-squares procedures to final R = 0.0650 and wR = 0.1719 using 2493 reflections. The imidazole ring is planar and the n-butyl chain adopts an extended conformation. The molecules in the crystal are stabilized by N–H s N type of intermolecular hydrogen bondings in addition to van der Waals forces. 相似文献
20.
Franz Pertlik Werner Mikenda Erich Steinwender 《Journal of chemical crystallography》1993,23(5):389-395
X-ray structural data are reported for 2,6-dimethyl-piperidinium-2-hydroxybenzoate (C14H21NO3, orthorhombic,P2121,21, (19);a=7.983(1)Å,b=12.680(2)Å,c=13.838(2)Å;Z=4;R=0.042) and for two polymorphs of 2,6-dimethylpiperidinium-2-hydroxythiobenzoate (C14H21NO2S), an-form (monoclinic,P21/n (14);a=8.005(4)Å,b=22.150(2)Å,c=8.672(4)Å,=101.91(6)°;Z=4;R=0.059) with an intramolecular O-HS hydrogen bond, and a-form (orthorhombic,P212121 (19);a=8.188(1)Å,b=14.781(2)Å,c=24.163(4)Å;Z=8;R=0.15) with an intramolecular O-HO hydrogen bond. The intra-and intermolecular hydrogen bond patterns are discussed, including the literature data of 2,6-dimethylpiperidinium-2-hydroxydithiobenzoate. 相似文献