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1.
The title compounds, [H3O+·18-crown-6][FeCl
4
–
] (1), and [H3O+·18-crown-6]2[CoCl
4
2–
] (2), were prepared by air oxidation of Fe(CO)5 for1, and Co2(CO)8 for2, in the presence of 18-crown-6, H2O and HCl(g) in toluene. Liquid clathrates formed immediately for both species:1·4.3 C7H8 and2·3.7 C7H8.1 crystallizes in the orthorhombic space group P21ma witha=10.357(1),b=11.824(1),c=8.961(1) Å, andD
c=1.46 g cm–3 forZ=2. Refinement based on 935 observed reflections led to a finalR value of 0.089.2 crystallizes in the monoclinic space group C2/c witha=16.225(1),b=11.522(1),c=20.136(1)Å, =97.75(2)o, andD
c=1.37 g cm–3 forZ=4. Refinement based on 1322 observed reflections led to a finalR value of 0.11. 相似文献
2.
The structures of anionic pyridine-2,6-dicarboxylato (pdc2–) complexes of cobalt, nickel, and copper have been studied. The stoichiometries and structures are very much dependent on whether KOH, Et4NOH, or NaOH is used in the synthesis to deprotonate the H2pdc ligand. Crystallographic results are: (1) K2[Co(pdc)2] · 7H2O, orthorhombic, Pnna, Z = 4, a = 20.637(2)Å, b = 13.480(1)Å, c = 8.200(1)Å (2) K2[Ni(pdc)2] · 7H2O, orthorhombic, Pnna, Z = 4, a = 20.648(1)Å, b = 13.375(1)Å, c = 8.2393(8)Å (3) [Co2(H2O)5(pdc)2] · 2H2O, monoclinic, P21/c, Z = 4, a = 8.3880(6)Å, b = 27.384(2)Å, c = 9.6110(8)Å, = 98.271(6)° (4) [Ni(Hpdc)2] · 3H2O, monoclinic, P21/c, Z = 4, a = 13.679(1)Å, b = 10.0450(9)Å, c = 13.767(2)Å, = 115.184(7)° (5) Na6[Co(H2O)6][Co(pdc)2]4 · 28H2O, monoclinic, P21/n, Z = 2, a = 13.363(1)Å, b = 8.437(1)Å, c = 40.689(3)Å, = 91.288(5)° (6) Na[Ni(Hpdc)(pdc)] · 11.5H2O, monoclinic, C2/m, Z = 4, a = 15.200(2)Å, b = 22.299(2)Å, c = 8.3596(7)Å, = 118.894(7)° (7) Na[Cu(Hpdc)(pdc)] · 3H2O, monoclinic, P21/n, Z = 4, a = 9.516(4)Å, b = 14.917(6)Å, c = 12.247(5)Å, = 92.00(5)°. The potassium and sodium complexes have extensive K+—H2O and Na+—H2O networks. The fact the Et4N+ ion does not appear in any of the complexes is likely due to the fact that it is incapable of forming the intricate cation—water and hydrogen-bonding networks observed in all of the other structures. 相似文献
3.
Chemical preparation, X-ray single crystal, thermal analysis, and IR spectrometric investigation of C4H14N2SO4·H2O (denoted DAMPS) are described. DAMPS crystallizes in the orthorhombic system with P212121 space group, a = 9.2726(4) Å, b = 9.5227(2) Å, c = 10.3807(4) Å, V = 916.62(6) Å3, and Z = 4. The DAMPS structure is built up from inorganic chains parallel to the b axis and linked via Ow–H···O hydrogen bonds. These chains are interconnected by organic groups so as to build a three-dimensional arrangement. 相似文献
4.
The structure of C6Cl5O–·C7H13NH+ has been determined by X-ray diffraction. The crystals are orthorhombic:Pcab,a=10.706(1),b=11.966(2),c=24.913(5)Å,Z=8. The structure was solved by direct methods, and refined to R=0.042 for 1523 nonzero reflections. The N+-HO– hydrogen bond is shortened (2.553(5)Å) and deformed (相似文献
5.
Sandra Ianelli Corrado Pelizzi Giancarlo Pelizzi Pieralberto Tarasconi 《Journal of chemical crystallography》1996,26(3):195-201
Manganese(II), nickel(II), and copper(II) complexes of 2,6-diacetylpyridine bis (acetylhydrazone) (H2dapac) have been synthesized and structurally characterized by X-ray diffraction methods. [Mn(H2dapac) (OH2)2](NO3)2 crystallizes in the monoclinic space groupP21/c witha=11.145(3),b=10.723(4),c=17.189(2) Å, =92.81(2)° andZ=4; [Ni(H2dapac)(OH2)2] (NO3)2·H2O crystallizes in the monoclinic space groupP21 witha=9.994(3),b=14.423(4),c=7.697(2)Å, =100.37(2)°, andZ=2; [Cu(H2dapac)(OH2)2](NO3)2·H2O crystallizes in the orthorhombic space groupPbcn witha=20.986(5),b=14.552(3),c=6.905(1)Å andZ=4. In each case the metal atom has a slightly distorted pentagonal bipyramidal environment, the equatorial positions being occupied by three nitrogen and two oxygen atoms from the hydrazone ligand and the apices by two water molecules. The crystalline cohesion in ensured by a three-dimensional network of hydrogen bonds involving the complex cations, the nitrate anions, and, where present, the uncoordinate water molecules. 相似文献
6.
Ilmarie Rencken Jan C. A. Boeyens S. Walter Orchard 《Journal of chemical crystallography》1988,18(3):293-306
The crystal and molecular structures of the title compounds CuCl·C8H14 and AgNO3·C8H14, have been determined by single-crystal X-ray diffraction techniques, and refined by full-matrix least squares. Both compounds crystallize in the orthorhombic space groupPbca witha=6.191(7),b=12.456(2),c=23.272(4) Å for CuCl·C8H14, anda=7.383(2),b=9.825(2),c=26.980(5) Å for AgNO3·C8H14;Z=8 in both cases. FinalR factors are 0.047 and 0.029 respectively. The cyclooctene ring has the twist chair-chair (TCC) conformation, with approximateD
2 symmetry, in both compounds, and the torsion angles around the double bonds are –134.2(4) and –137.0(4)° respectively. Slight lengthening of the metal-complexed double bond is attributed to enhanced olefin metal -donation of thetrans bond. 相似文献
7.
Kurt Mereiter Werner Mikenda Erich Steinwender 《Journal of chemical crystallography》1993,23(5):397-402
X-ray structural data are reported for tetraethylammonium-2-hydroxythiobenzoate (C15H25NO2S; orthorhombic,Pna21(33);a=14.155(2)Å,b=7.651(1)Å,c=14.855(2)Å;Z=4;R=0.038, at 295 K) and for tetraethylammonium-2-hydroxydithiobenzoate (C15H25NOS2; orthorhombic,Pna21(33);a=15.668(4)Å,b=8.729(2)Å,c=12.350(3)Å;Z=4;R=0.031, at 295 K). In both compounds the OH groups are engaged in intramolecular O-HS hydrogen bonds (OS=2.88 and 2.89 Å, respectively). 相似文献
8.
G. C. Rout M. Seshasayee G. Aravamudan K. Radha 《Journal of chemical crystallography》1984,14(2):193-204
The synthesis, properties, and structural characterization of the title compound, C16H30N4O4S7Te(IV)·H2O, are reported. The crystals are monoclinic, space groupP21/n, withZ=4 in a unit cell of dimensionsa=13.291(5),b=21.306(6),c=10.450(1) Å, 0=104.25(2)° and,V
c=2868 Å3. The structure was solved by the heavy atom method and refined by full-matrix least squares toR=0.025 andR
w
=0.027 for 2894 reflections. The dithiocarbamate groups are linked in an unequal bidentate manner with Te-S average distance 2.695(1) Å. The thiocyanate group is bonded through the sulfur atom with much larger Te-S length [2.964(2) Å]. 相似文献
9.
C. G. Vonk 《Journal of chemical crystallography》1973,3(4):201-207
The structure of crystals of the composition Zn[Cl2Ti(C5H5)2]2·2C6H6 has been determined from Patterson and Fourier syntheses of two projections, and refined toR = 0·117 by full-matrix three-dimensional least-squares methods. The crystals are orthorhombic:Pbcn,a = 18·45(5),b = 15·40(6),c = 11·35(3) Å,Z= 4. The complex consists of a central distorted ZnCl
4
2–
tetrahedron linked along the Cl—Cl edges to two distorted TiCl2(C5H5)2
+ tetrahedra in such a way that their centres are nearly collinear The two C6H6 molecules in the formulae unit may be regarded as benzene of crystallization. 相似文献
10.
Veronique Gibon Kristina Szafraniak Guy Evrard Francois Durant 《Journal of chemical crystallography》1987,17(6):751-760
The crystal structure of oxacillin sulfone has been determined by single-crystal X-ray diffraction techniques and refined by full-matrix least squares. The penicillin molecule cocrystallizes with H2O in an orthorhombic space groupP212121 witha=10.303(7) Å,b=26.735(17) Å, andc=7.384(4) Å. The calculated density is 1.526 g cm–3, with aZ value of 4. FinalR-factor is 0.035. The oxidation of the sulfur atom is discussed in terms ofS1 conformation of the penam moiety and in terms of hydrogen-bond formation between one oxygen of the sulfur atom and the amidic hydrogen of the C6 side-chain. A comparison with oxacillin and cloxacillin sulfoxide is also made. 相似文献
11.
The crystalline dihydrate and hydrochloride trihydrate of a new betaine, namely, L·2H2O (1) and [L2H]Cl·3H2O(2) (L=p-Me2NC5H4N+CH2CO2), have been synthesized and characterized by X-ray crystallography. Molecule L in compound1 [space groupPbcn, witha=15.732(3),b=7.894(2),c=18.304(4) Å, andZ=8] possesses approximateC
s
symmetry. The formation of hydrogen bonds by water molecules bridging neighboring carboxy oxygen atoms leads to an infinite two-dimensional network composed of a packing of two different kinds of 12-membered rings. In compound2 [space group PT witha=7.341(2),b=9.543(2),c=17.010(4) Å, =82.43(2)°, =80.34(2)°, =74.05(2)°, andZ=2], the carboxylate groups of a pair of betaine molecules are bridged by a proton to form a dimeric cation L2H+ with a very strong asymmetric hydrogen bond of length 2.464(7) Å. The crystal structure features a hydrogen-bonded corrugated ribbon comprising an alternate arrangement of edge-sharing centrosymmetric (H2O)4(Cl–)2 and (H2O)4 rings running parallel to thea axis. 相似文献
12.
Jerry L. Atwood Simon G. Bott Kerry D. Robinson Elizabeth J. Bishop Michael T. May 《Journal of chemical crystallography》1991,21(4):459-462
The title compound was synthesized by the reaction of [H3O+·18-crown-6][Cl-H-Cl–]·3.8 C6H5Me with two equivalents of H2O. Colorless crystals, which slowly deposited from the corresponding liquid clathrate, belong to the monoclinic space group P21/n witha=10.648(6),b=9.571(2),c=20.801(6) Å,=98.67(5)°, andD
c=1.24 g cm–3 forZ=4. Refinement based on 1609 observed reflections led to a finalR value of 0.072. In the crystal structure the [H3O+·18-crown-6]+ cations are packed in layers separated by puckered sheets of [(H5O
2
+
)(Cl–)2]–. 相似文献
13.
The crystal structures of (i) CH3(C9H6O2)SO2C6H5 and (ii) CH3(C8H8O2)SO2−C6H5 have been determined by X-ray diffraction. (i) crystallizes in the monoclinic space groupP21/c with unit cell parametersa=8.814(1)?,b=10.310(1)?,c=15.841(4)?, β=98.17(1)o, andZ=4, and (ii) crystallizes in the orthorhombic space groupP212121 with unit cell parametersa=6.206(1)?,b=11.752(5)?,c=19.865(3)?, andZ=4. The pyran ring in both of them is in the distorted half-chair conformation with differeing degrees of distortion from
the ideal. 相似文献
14.
The 5-hexyl (I) and the 5-heptyl (II) analogs of 2,4-diamino-6-methylpyrimidine both crystallize in the space groupP21/c withZ=4. Unit cell parameters of I are C11H20N4·H2O,a=17.204(3),b=4.609(9),c=16.765(2)Å,= 91.53(2)°; those of II are C12H23N4
+·C2H5SO3
–,a=12.489(1),b=16.702(2),c=8.9558(7)Å,=99.208(8)°. The molecular packing of I contains one water, while II forms a salt with ethanesulfonic acid. The alkyl chain of I adopts an alltrans conformation; in contrast, II has onegauche orientation between carbons 2 and 3 of heptyl. These are the first structural data on two alkyl lipophilic antifolates with antineoplastic activity. 相似文献
15.
C30H51NO4P2Pt-[C2H3N], orthorhombic,Pbca, a=16.132(1),b=16.610(2),c=24.001(2) Å.Z=8,D
c=1.54 g cm–3,R=0.042,R
w=0.048, GOF=1.33. The platinaoxalate (PtC2O2) ring fragment is essentially planar with Pt–O bond lengths of 2.067(8) and 2.058(7) Å. 相似文献
16.
W. K. L. Van Havere Paul T. Beurskens A. T. H. Lenstra 《Journal of chemical crystallography》1985,15(1):45-52
The crystal structure of bis(potassium hydrogenl-malate)·malic acid, 2[K+(C4H5O5)–]·C4H6O5, has been determined: C12H16K2O15, M
r
=1913.9, orthorhombic, space groupP212121
a=7.719(5),b=7.916(5),c=29.863(20) Å,V
c=1824.7 Å3,Z=4. The structure was determined by a new application of theDirdif procedure using MoK automatic diffractometer X-ray data, and refined by full-matrix least squares toR=0.059 for 962 reflections. A question on space-group assignment and composition was resolved only after the structure had been determined. The conformation of the central carbon skeleton of all three crystallographic independent malate moieties isanti. The potassium ions are coordinated by eight oxygen atoms, forming face-sharing distorted square antiprisms. 相似文献
17.
Andrzej Fruziński Janina Karolak-Wojciechowska Sandrine Alibert-Franco Christiane Santelli-Rouvier Jacques Barbe 《Journal of chemical crystallography》1999,29(11):1201-1204
As a part of studies on MDR reversing agents, the structure of a benzylamido-9,10-dihydro-9,10-ethenoanthracene is reported: C24 H19 N O; orthorhombic; space group: Pca21; a = 9.214(2), b = 18.624(4), c = 10.170(2) Å; 1745.2(6) Å3; Z = 4. The three nonplanar rings from the 9,10-dihydro-9,10-ethenoanthracene skeleton of the molecule adopt a boat conformation. The benzamide side-chain is extended (conformation, trans-trans-gauche). The molecules in the crystal are joined by infinite chains of H-bonds N14–H14···O13. 相似文献
18.
L. Golič I. Leban S. Detoni B. Orel D. Hadži 《Journal of chemical crystallography》1985,15(3):215-228
From an equimolar mixture of guanidine and maleic acid, two different crystal modifications of guanidinium hydrogen maleate, CH6N
3
+
·C4H3O
4
–
, were isolated and their crystal structures determined using three-dimensional diffractometer data. Crystals of both forms are orthorhombic:Pca21,a=19.012(8)b=3.758(1),c=11.119(5) Å,Z=4 for form I;Fdd2,a=18.505(2),b=20.007(3),c=8.406(2) Å,Z=16 for form II. The structures were solved by direct methods and refined by full-matrix least squares to conventionalR values of 0.064 for form I and 0.043 for form II, with 488 and 605 reflections respectively. The structures consist of planar guanidinium cations C(NH2)
3
+
and hydrogen-maleate residues C4H3O
4
–
. There are no significant differences in distances and angles within the guanidinium and hydrogen-maleate units. However, a substantial difference appears in the length and geometry of the intramolecular hydrogen bond OHO. The packing of cations and anions is also completely different in the two forms. Infrared and Raman spectra of the title compound are presented, and salient differences between them and the spectrum of the symmetrically bonded potassium hydrogen maleate are discussed briefly. 相似文献
19.
Frans G. Moers Sandip K. Nayak René de Gelder Jan M.M. Smits Lambertus Thijs Binne Zwanenburg 《Journal of chemical crystallography》1999,29(9):1053-1056
The crystal and molecular structure of 2-{(R)-1-Hydroxy-1-[(2S)-1-tritylaziridin-2-y1] methy1}acrylate is described. Crystal data: C26H25NO3, orthorhombic, space group P212121, a = 9.6954(5), b = 13.1458(5), c = 16.7885(7) Å, V = 2139.8(2) Å3, Z = 4. The (R,S) diastereomer shows an intramolecular hydrogen bonding N···H—O under formation of a five-membered ring with N···O distance of 2.664 Å. IR, 1H NMR and 13C NMR data are discussed. The 1H NMR of the (R,S) diastereomer shows a singlet- whereas the (S,S) diastereomer exhibits a doublet-pattern for the hydroxyl proton. 相似文献
20.
Rubidium and ammonium hydrogen glutarates (M
+
–CO2.C3H6.CO2H) each crystallize with four molecules in orthorhombic unit cells of almost identical dimensions: (M = Rb)a = 18·55,b = 7·57,c = 5·29 Å; (M = NH4)a= 18·59,b= 7·56,c= 5· 27 Å. They have very similar structures, but they are not isomorphous: space groupsCmma (Rb) andPmaa (NH4).The crystal structures have been determined by three-dimensional X-ray analysis and refined with moderate precision. Both have infinite chains of glutarate residues, linked end-to-end by very short, symmetrical hydrogen bonds, with O···H···O = 2·40(2) (Rb) and O···H···O = 2·460(6) Å (NH4).In the Rb salt, the glutarate residue has strict, crystallographicm symmetry. The difference in the NH4 salt arises from small movements of the carbon and (especially) the oxygen atoms out of this symmetry plane. These are due to N-H···O bonding: two equivalent cations in the Rb salt, each making contact with eight oxygen atoms, become differentiated in the NH4 salt by linkage to different sets of four oxygens.We wish to acknowledge financial support from the Science Research Council, and our indebtedness to Drs. J. G. Sime, K. W. Muir and others for help with KDF9 programs. 相似文献