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1.
Abdelhamid Mousser Abdelaziz Bennouna Abdelaziz Gorfti Michèle Salmain Claude Cabestaing Gérard Jaouen 《Journal of chemical crystallography》1996,26(12):835-840
The crystal structures of [(5-C5H4COOH)W(CO)3R] (R=Me, I) have been determined. They crystallize in two different monoclinic space groups. R=Me isP21/c,a=10.4833(6),b=8.0144(7),c=13.0731(6) , =93.147(4)°, andD(calc)=2.374 g-cm–3 forZ=4. R=I isP21/n,a=7.814(2),b=13.075(4),c=11.097(4) , =91.75(2)°, andD(calc)=2.953 g-cm–3 forZ=4. Both possess a four-legged piano stool geometry. The methyl ligand in the R=Me complex is disordered between two positions insyn oranti relative to the substituted carbon of the cyclopentadienyl ligand. The iodo ligand in the R=I complex is, however, exclusively insyn-position. 相似文献
2.
Ian R. Butler Jean -Louis Roustan Jean -Pierre Charland 《Journal of chemical crystallography》1990,20(4):335-338
Protonation of Fe(
5-C5H5)[(
5-C5H4)(2-C5H4N)]1 in 98% H2SO4 followed by dilution with water and addition of NaBF4 yields Fe(
5-C5H5)[(
5-C5H4)(2-C5H4NH+)](BF
4
–
)2 instead of a ferrocinium derivative. Complex2 crystallizes in the monoclinic system, P21 /a:a=7.984(1),b=9.981(2),c=18.220(4) Å,=102.31 (1)°,V=1418.5 Å3,Z=4. The pyridinium ring makes a dihedral angle of 21.0(2)° with the cyclopentadienyl ring to which it is bound. One F atom of BF
4
–
is involved in short van der Walls contacts with the N (2.764(5) Å) and the H (2.08(6) Å) atoms of the NH+ moiety. 相似文献
3.
Joanna K. Day Amber L. Thompson Simon Aldridge 《Journal of chemical crystallography》2010,40(2):156-159
4.
Peter Johnston Louis Denner Charles F. Marais Jan C. A. Boeyens Neil J. Coville 《Journal of chemical crystallography》1988,18(4):403-428
The crystal and molecular structures of three derivatives of [(
5-C5H4Me)Fe(CO)(L)I] [L=2,6-Me2C6H3NC, P(OMe)3, and P(C6H11)3] have been determined. [(
5-C5H4Me)Fe(CO)(CNC6H3Me2-2,6)I] (1): Space groupP¯1,Z=2,a=13.193(7),b=8.183(5),c=7.465(4) Å,=95.13(5),=94.39(5), =91.09(5)°. [(
5-C5H4Me)Fe(CO)[P(OMe)3]I] (2): Space groupP21/c,Z=4,a=7.296(3),b=24.471(6),c=8.877(3) Å,=111.92(4)°. [(
5-C5H4Me)Fe(CO)[P(C6H11)3]I] (3): Space groupP21/c,Z=4,a=9.809(3),b=14.147(2),c=8.276(3) Å,=103.07(2)°. The structures were refined toR values of 0.045, 0.070, and 0.061, respectively. Disorder was observed in the P(OMe)3 ligands on2. Structural data for1 and3 reveal (i) a small movement of the Fe atom away from the ringC atom containing the methyl group, (ii) a larger movement of ring C atoms away from the ring least-squares plane for3 than for1, and (iii) a shift toward an allyl-ene bond length variation in the ring distances for3. Molecular mechanics calculations performed on2 produce a low-energy conformation similar to that found in the crystal structure determination of2 with an energy barrier to ring rotation of ±5 kcal mol–1. A correlation of the structural and molecular mechanics data with the nmr spectra of complexes1 to3 indicates that the steric influence ofL on the ring rotation could be due to ring distortion and/or interaction with the ring methyl group. 相似文献
5.
Zhong -Wu Guo A. Zamojski J. W. Krajewski P. Gluziński 《Journal of chemical crystallography》1993,23(3):209-221
Conformational analysis of the alkylation and aldol condensation products of phenylacetyliron complex (4), based on1H-NMR chemical shifts and1H-1H vicinal coupling constants, permitted the assignment of relative configurations to all products obtained. Configurations and conformations of two aldol condensation products,12A and13F, were determined by X-ray structural analysis and were compared with the structures deduced from1H-NMR data. The crystals of12A and13F are monoclinic, space group of12A isP21/n with cell dimensions:a=10.937(2),b=17.278(5),c=16.412(3)Å, andβ=107.52(2)°; space group of13F isP21/c, with cell dimensions:a=11.576(4),b=21.180(2),c=11.854(4)Å, andβ=99.80(3)°. Both structures were solved by direct methods, and refined by a full-matrix, least-squares procedure giving for12A R=0.0599 and for13F R=0.0459. 相似文献
6.
Simon Aldridge Richard J. Calder Simon J. Coles Michael B. Hursthouse 《Journal of chemical crystallography》2003,33(10):805-808
The organometallic zwitterion (5-C5H3MeBCl3)Fe(CO)3 (2) is isolated as a minor product from the reaction between the sodium salt of the anion [(5-C5H4Me)Fe(CO)2]– and boron trichloride. The crystal structure of 2 [P21/n, a = 7.3927(5) Å, b = 13.8027(9) Å, c = 12.2759(9) Å, = = 90°, = 92.517(3)°] features discrete molecules in which the coordination sphere of the iron center comprises three carbonyls and a novel ( 5-C5H3MeBCl3) ligand, derived from attack of BCl3 on the ( 5-C5H4Me) moiety of the parent compound. The isolation of 2 confirms that the nucleophilic properties of organometallic anions of the type [( 5-C5R5)M(CO)
n
]– (M = Fe, Ru, n = 2; M = Mo, W, n = 3) are not confined to the metal center, or to the carbonyl oxygens (examples of which have previously been reported) but also encompass the cyclopentadienyl ligand. 相似文献
7.
The crystal structure of the complex [Pd(
5-C5 H5) (PPh2) CH2CH2PPh2]+ [CF3SO3]– has been determined from single crystal X-ray data and refined by least-squares methods toR=0.046. The monoclinic crystals have unit cell dimensionsa=9.832(3),b=12.104(4),c=13.765(4)Å,=111.22(3)°, space group P21, andz=2. In the cationic complex the palladium atom is coordinated to the
5-cyclopentadienyl moiety and to the phoshorus atoms of the chelating diphosphine. The arrangement of the two phosphorus atoms and the centroid of the cyclopentadienyl ring is approximately trigonal. 相似文献
8.
J. W. Krajewski P. Gluziński A. Zamojski A. Mishnyov A. Kemme Zhong-Wu Guo 《Journal of chemical crystallography》1992,22(2):213-217
The crystal and molecular structure of cyclopentadienyl-carbonyl-triphenylphosphine-phenylacetyl-iron (1) has been determined on the basis of X-ray data. The crystals are triclinic, space groupP¯1 (Z=2) with cell dimensions:a=9.546(1),b=10.233(1),c=5.012(2) Å,=93.70(1),=101.12(1), =112.58(1)°. The structure was solved by direct methods and refined anisotropically by a full-matrix, least-squares procedure against 4964 independent reflections, givingR=0.0416. The MM calculations done for a model of1 reproduced satisfactorily the X-ray structure.On leave from the Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, China. 相似文献
9.
Jan C. A. Boeyens Lin Cheng Neil J. Coville Demetrius C. Levendis Keith McIntosh 《Journal of chemical crystallography》1998,28(3):185-191
Single crystal X-ray structures of diag and lat-(5-C5H4Me)Re(CO)2Br2 have been determined. The diag form crystallizes in the triclinic space group
, a = 6.751(2), b = 8.537(1), c = 9.758(1) Å = 96.70(1), = 93.15(2), = 104.96(2)°, V = 534.8(2) Å3, Z = 2. The lat form is monoclinic, P21/c, a = 11.820(1), b = 7.133(1), c = 12.924(1) Å = 98.278(8)°, V = 1078.2(2) Å3, Z = 4. The unit cell volumes (per Z) of the two isomers differ by ca 1%. Molecular modelling reveals an energy difference between the two isomers of 1 kJ mol–1 or less. The XRD powder diffraction patterns for the lat isomer produced by crystallization from solution or prepared by thermal isomerization are identical. The evidence thus suggests that the solid state isomerization reaction is a novel example of a reaction which yields a molecular structure determined by crystal packing forces. 相似文献
10.
Melvyn Rowen Churchill Charles H. Lake Lisa F. Szczepura Kenneth J. Takeuchi 《Journal of chemical crystallography》1996,26(7):489-495
The title complex crystallizes in the centrosymmetric monoclinic space group C2/c (No. 15) withZ=8. The structure was refined toR=4.49% for those 2745 independent reflections with 2=5–50o and |F
|>6(F). Ruthenium-ligand distances are as follows: Ru-P=2.284(2) and 2.286(2) Å, Ru-NO2=2.049(6) Å and Ru-C(Cp)=2.210(10)-2.246(9) Å. Bond lengths within the nitro ligand are N(1)-O(1)=1.226(10) Å and N(1)-O(2)=1.244(10) Å. The methanol of solvation is ordered but is subject to large thermal vibrational motions. 相似文献
11.
J. W. Krajewski P. Gluziński A. Zamojski A. Mishnyov A. Kemme Guo Zhong-Wu 《Journal of chemical crystallography》1991,21(3):271-275
The crystal and molecular structure of cyclopentadienyl-carbonyl-triphenylphosphine-methoxy-acetyl-iron (2) has been determined by X-ray. The crystals are monoclinic:P21/n,Z=4,=7.881(1),b=19.111(3),c=15.271(2) Å and=93.44(1)°. The structure was solved by direct methods, and refined anisotropically by full-matrix least-squares against 3419 independent reflections, givingR=0.0446. Molecular mechanics calculations reproduce satisfactorily the X-ray structure.On leave from the Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai, China. 相似文献
12.
The crystal structure of 1,1′-di-tert-butylnickelocene is studied by the X-ray diffraction technique in the temperature range 143–243 K. The crystals are monoclinic, space group P21/n, Z = 2. The molecule is centrosymmetric. The cyclic ligands are parallel and adopt a staggered conformation. At 143 K, the mean bond lengths are as follows: Ni-C, 2.194(6); C-C (in the ring), 1.421(6); and C-C (Me), 1.538(2) Å. Analysis of the thermal motion of the molecule is performed within the single-parameter model, which allows for the independent motion of the cyclopentadienyl ring with the tert-butyl group as a whole and the motion of the tert-butyl group. It is shown that the molecule is structurally nonrigid and the tert-butyl group executes librational motion. The B 5 heights of the rotation barriers are estimated from the rms libration amplitudes: 〈?2〉 are equal to 40(5) and 34(4) kJ/mol at 143 and 243 K, respectively. 相似文献
13.
14.
Khandakar M. Hanif Mohammad S. Islam Shariff E. Kabir K. M. Abdul Malik Md. Arzu Miah Nathan Wakelin 《Journal of chemical crystallography》2003,33(11):859-865
Treatment of Ru3(CO)12 with 2-mercaptobenzothiazole at 68°C gave the known compound [(-H)Ru3(3-2-C7H4NS2)(CO)9] 1 and the new compound [(-H)2Ru3(-2-C
7H4NS2) (3-2-C7H4NS2)(CO)7] 2 in 15 and 10% yields respectively. Compound 2 has been characterized by elemental analysis, infrared, 1H NMR and mass spectroscopic data together with single crystal X-ray crystallography. It crystallizes in the monoclinic space group C2/c with a = 31.662(6), b = 14.577(3), c = 11.602(2) Å, = 104.15(3)°, Z = 8, and V = 5192.4(2) Å3. The compound consists of a Ru3 triangle with three different Ru-Ru bond lengths [2.75264, 2.79084, 2.97604 Å] and the two 2-mercaptobenzothiazole ligands are differently attached to the metal atoms. Compound 2 is also obtained by the reaction of 1 with excess 2-mercaptobenzothiazole at 68°C. 相似文献
15.
Christoph Balzarek David R. Tyler Timothy J. R. Weakley 《Journal of chemical crystallography》2002,32(7):161-163
The compound bis(5-methylcyclopentadienyl)-bis(4-methylbenzenesulfonato-O)-molybdenum (IV) crystallizes in space-group P21/c, a = 8.2956(5), b = 26.896(3), c = 11.4196(11) Å, = 96.101(7)°, Z = 4. The sulfonate ligands are monodentate and the molybdenum atom has pseudotetrahedral coordination geometry, with angles O–Mo–O 72.0(1)° and Cp–Mo–Cp 134.9(1)° (Cp = ring centroid). 相似文献
16.
Francisco Hueso-Ureña Sonia B. Jiménez-Pulido Miguel N. Moreno-Carretero Miguel Quirós-Olozábal Juan M. Salas-Peregrín 《Journal of chemical crystallography》1999,29(5):571-574
Single-crystal X-ray diffraction studies have been performed on the complex cis-diaqua-bis(1,3-dimethylpteridine-2,4(1H,3H)-dione-O4,N5) copper(II) perchlorate monohydrate, [Cu(DLM)2(H2O)2](ClO4)2 · H2O. This compound crystallizes in the orthorhombic system, P212121 space group, Z = 4 with a = 8.749(1) Å, b = 14.213(1) Å, c = 21.200(2) Å, and V = 2636.2(4) Å3. The metal ion is surrounded in octahedral geometry by two mutually quasi-perpendicular N5,O4-coordinated lumazine chelators with the O4 atoms trans and the N5 atoms cis. The polyhedron is completed by two cis-coordinated water molecules. The absolute configuration of the complex can be described, following Bailar's nomenclature, as the enantiomer of the stereoisomer 4M. A three-dimensional hydrogen-bond network is defined by water molecules, perchlorate anions, and the O2 of the pteridine A. 相似文献
17.
Gilbert J. Matare Kevin M. Kane Pamela J. Shapiro Ashwani Vij 《Journal of chemical crystallography》1998,28(10):731-734
cis-[(1,2-diphenyl-1,2-dicyclopentadienyl)ethanediyl]bis(tetrahydrofuran)calcium is prepared by reductively coupling phenylfulvene with activated calcium to produce cis and trans isomers which can be separately crystallized. The cis isomer crystallizes in the monoclinic space group P21/c. The cell parameters are: a = 9.7006(1), b = 18.9839(1), c = 14.2018(2) Å, = 91.263(1)°, V = 2614.70(5) Å3, D
calc = 1.252 mg/m3, and Z = 4. Spectroscopic and crystallographic data for the cis-isomer are presented and discussed. 相似文献
18.
A. B. Ilyukhin R. L. Davidovich I. N. Samsonova L. V. Teplukhina 《Crystallography Reports》2000,45(1):39-43
The crystal structures of K[M(Dtpa)] ? 3H2O (M = Zr or Hf) and NH4[Sn(Dtpa)] ? H2O are studied by X-ray diffraction. The coordination number of the metal atom in all the compounds is eight. The NH4[Sn(Dtpa)] ? H2O complex is isostructural to the (H5O2)[M(Dtpa)] ? H2O (M = Sn or Hf) compounds studied earlier. 相似文献
19.
20.
Kazi A. Azam Anjoli R. Das Michael B. Hursthouse Shariff E. Kabir K. M. Abdul Malik 《Journal of chemical crystallography》1998,28(4):283-288
The reaction of [Os3(CO)10(MeCN)2] with 2-ethylpyridine at ambient temperature leads to the isolation of the cluster [(-H)Os3(CO)10(-2-N=CCH=CHCH=CC2H5)][3 (65% yield) which has been structurally characterized by crystallographic methods. The compound crystallizes in the triclinic space group
with a = 9.334(2), b = 9.918(2), c = 11.767(1) Å, = 92.13(2), = 99.93(1), = 99.88(2)°, V = 1054.7(3) Å3 and Z = 2. The same edge of the osmium triangle in the cluster is bridged by both the hydrido and the heterocyclic ligands, the latter through the nitrogen and the carbon atoms of the C=N bond. 相似文献