Short Sn Research Articles

The crystal structures of tritin(II) bromide pentafluoride and ditin(II) chloride trifluoride

The crystal structures of the title compounds have been determined from X-ray photographic data by Patterson and Fourier methods. The crystals of both compounds have pseudo-high-symmetry cells but Sn3BrF5 is monoclinic with space group P21/n and Z= 4 in a unit cell of dimensions a= 4.27, b= 12.70, c= 12.70 A, β= 90.0°, and Sn2ClF3 is orthorhombic with space group P212121 and Z= 4 in a unit cell of dimensions a=b=c= 7.88 A. Both structures contain infinite tin–fluorine cationic networks in which all the tin atoms have a trigonal pyramidal co-ordination of nearest-neighbour fluorine atoms. The shortest Sn–Br (3.29 A) and Sn–Cl (3.14 A) distances are consistent with the presence of free Br– and Cl– ions in the lattices.

ChemInform Abstract: CRYSTAL AND MOLECULAR STRUCTURE OF QUINOLINIUM TRICHLORODIMETHYLSTANNATE(IV)

Chemischer InformationsdienstVolume 7, Issue 4 Organoelement Compounds ChemInform Abstract: CRYSTAL AND MOLECULAR STRUCTURE OF QUINOLINIUM TRICHLORODIMETHYLSTANNATE(IV) A. JULIET BUTTENSHAW, A. JULIET BUTTENSHAWSearch for more papers by this authorMICHAEL DUCHENE, MICHAEL DUCHENESearch for more papers by this authorMICHAEL WEBSTER, MICHAEL WEBSTERSearch for more papers by this author A. JULIET BUTTENSHAW, A. JULIET BUTTENSHAWSearch for more papers by this authorMICHAEL DUCHENE, MICHAEL DUCHENESearch for more papers by this authorMICHAEL WEBSTER, MICHAEL WEBSTERSearch for more papers by this author First published: January 27, 1976 https://doi.org/10.1002/chin.197604255AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article. Volume7, Issue4January 27, 1976 RelatedInformation

Sn+ Centers in KCl:SnCl2

physica status solidi (b)Volume 71, Issue 1 p. K81-K85 Short Note Sn+ Centers in KCl:SnCl2† C. J. Delbecq, C. J. Delbecq Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this authorR. Hartford, R. Hartford Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this authorD. Schoemaker, D. Schoemaker Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this authorP. H. Yuster, P. H. Yuster Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this author C. J. Delbecq, C. J. Delbecq Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this authorR. Hartford, R. Hartford Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this authorD. Schoemaker, D. Schoemaker Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this authorP. H. Yuster, P. H. Yuster Argonne National Laboratory, Argonne, IllinoisSearch for more papers by this author First published: 1 September 1975 https://doi.org/10.1002/pssb.2220710160Citations: 5 † Based on work performed under the auspices of the U. S. Energy Research and Development Administration. AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat Citing Literature Volume71, Issue11 September 1975Pages K81-K85 RelatedInformation

Crystal structure of tritin(II) dihydroxide oxide sulphate

The crystal structure of the title compound has been determined from X-ray diffractometer data by Patterson and Fourier methods. Crystals are orthorhombic and piezoelectric, space group Pbc21 with Z= 4 in a unit cell of dimensions a= 4.983 ± 0.002, b= 13.1 28 ± 0.005, c= 1 2.214 ± 0.005 A. The structure was refined by least-squares methods to R 0.028 for 1 070 reflections. The structure contains discrete ring [Sn3O(OH)2]2+ basic ions which have Sn in two different environments : one Sn is bonded to all three ring oxygens to give trigonal pyramidal co-ordination with short Sn–O, and the remaining Sn atoms are bonded to two ring O atoms with short Sn-O ( 2.40 A) distances. These latter Sn atoms have distorted square-pyramidal oxygen environments. The bonds between the SO4 groups and the basic ion Sn atoms result in the formation of a layer structure.

Crystal and molecular structure of quinolinium trichlorodimethylstannate(IV)

The structure of [C9H8N][Me2SnCl3] has been determined by single-crystal X-ray diffraction from photographic data by the heavy-atom method, and refined to R 5.5%. Crystals are triclinic, a= 9.55(3), b= 2.53(2), c= 7.03(2)A, α= 109.4(1), β 96.7(3), γ= 111.2(2)°, Z= 2, space group P. The anion, of approximate C2v symmetry, has a structure intermediate between a trigonal bipyramid and square pyramid. When based on the former, carbon atoms occupy equatorial positions [Sn–Cl 2.560(9). 2.585(9)(ax), 2.407(5)(eq), Sn–C 2.08(3)A, C–Sn–C 152.2(8)°] whilst with the latter description there is a short (2.407 A) Sn–Cl(ax) bond. There is a weak Sn ⋯ Cl interaction between atoms of adjacent anions, giving rise to dimeric units [Sn ⋯ Cl 3.486(7)A]. The geometry of the planar cation is as expected.

ChemInform Abstract: CRYSTAL STRUCTURE OF POLYMERIC TRIS(TRIMETHYLTIN)CHROMATE HYDROXIDE

Crystals of the title compound are orthorhombic, space group Pbca, a= 20·85(2), b= 11·55(2), c= 16·58(2)A(at ca. –30 °C), Z= 8. The structure was determined at ca. –30 °C from diffractometer data by direct methods and refined by full-matrix least-squares to R 0·045 for 488 unique observed reflexions. The structure consists of a complicated network polymer. There are three crystallographically independent and approximately planar tri-methyltin groups, and in each case, approximately trigonal bipyramidal co-ordination of the tin atom is completed by two axial oxygen atoms. Each oxygen atom in the chromate group is also bonded to tin, and the hydroxide group bridges two trimethyltin groups and is probably hydrogen bonded to one of the chromate oxygens. The two tin atoms linked by the hydroxide group have similar co-ordination geometries, with short Sn–O(H)[2.l4(3) and 2·17(4)A] and long Sn–O(Cr)[2·48(5) and 2·51(4)A]. The two oxygen atoms responsible for the long Sn–O bonds make the shortest two Cr–O bond lengths [1·61(4) and 1·56(4)A]. Other bond lengths and angles are : Sn–O, 2·16(4) and 2·29(4); Cr–O, 1·78(4) and 1·70(4); mean Sn–C, 2·13 A; mean C–Sn–C, 119; mean O–Sn–O, 176; mean Cr–O–Sn, 144; and Sn–O–Sn, 136(2)°.

Crystal structure of polymeric tris(trimethyltin) chromate hydroxide

Crystals of the title compound are orthorhombic, space group Pbca, a= 20·85(2), b= 11·55(2), c= 16·58(2)A(at ca. –30 °C), Z= 8. The structure was determined at ca. –30 °C from diffractometer data by direct methods and refined by full-matrix least-squares to R 0·045 for 488 unique observed reflexions. The structure consists of a complicated network polymer. There are three crystallographically independent and approximately planar tri-methyltin groups, and in each case, approximately trigonal bipyramidal co-ordination of the tin atom is completed by two axial oxygen atoms. Each oxygen atom in the chromate group is also bonded to tin, and the hydroxide group bridges two trimethyltin groups and is probably hydrogen bonded to one of the chromate oxygens. The two tin atoms linked by the hydroxide group have similar co-ordination geometries, with short Sn–O(H)[2.l4(3) and 2·17(4)A] and long Sn–O(Cr)[2·48(5) and 2·51(4)A]. The two oxygen atoms responsible for the long Sn–O bonds make the shortest two Cr–O bond lengths [1·61(4) and 1·56(4)A]. Other bond lengths and angles are : Sn–O, 2·16(4) and 2·29(4); Cr–O, 1·78(4) and 1·70(4); mean Sn–C, 2·13 A; mean C–Sn–C, 119; mean O–Sn–O, 176; mean Cr–O–Sn, 144; and Sn–O–Sn, 136(2)°.

Crystal structure of dichloro(diphenyl)tin

The crystal and molecular structure of dichloro(diphenyl)tin has been determined by single-crystal X-ray diffraction methods using the intensities of about 3800 reflections measured by counter diffractometry. The crystals belong to the triclinic system, a= 15·905(2), b= 9·367(1), c= 9·034(1)A, α= 76·89(1), β= 93·21(1), γ= 94·78(1)°, space group P, and Z= 4. The structure was solved by Patterson and Fourier methods and refined by block-diagonal least-squares techniques, using individual anisotropic thermal parameters, to R 0·040. All hydrogen atom positions were located but were not refined.There are two discrete molecules of Ph2SnCl2 in the asymmetric unit with identical geometry. The mean bond distances are: Sn–Cl 2·346(2), Sn–C 2·114(3), and C–C 1·387(13)A. Mean values for the valence angles at the tin atom are: Cl–Sn–Cl 100, Cl–Sn–C 107, and C–Sn–C, 125·5°.There is no molecular association in the crystal, the shortest Sn ⋯ Cl contact being 3·77 A. The interpretation of Mossbauer spectroscopic results in terms of a polymeric network in the crystal structure involving six-co-ordinate tin is thus shown to be incorrect.

The Mössbauer effect in tin(II) compounds. Part X. Insertion reactions of tin(II) compounds with carbonyl-π-cyclopentadienyliron derivatives

The products of the insertion reactions of a number of tin(II) compounds SnX2(X = Cl, Br, I, NCS, HCO2, and AcO) with [(π-C5H5)Fe(CO)2]2 and (π-C5H5)Fe(CO2)2Cl are compared with those from replacement of Cl from [(π-C5H5)Fe(CO)2]2·SnCl2 and (π-C5H5)Fe(CO)2SnCl3. The 119Sn Mossbauer parameters of both series of compounds [(π-C5H5)Fe(CO)2]2·SnX2 and (π-C5H5)Fe(CO)2·SnX3(X = Cl, Br, I, NCS, HCO2, and AcO) show that the use of tin bonding electrons is dominated by the Sn–Fe bond. The trends in chemical isomer shift and quadrupole splitting can be explained with reference to the very short Sn–Fe bond lengths in these materials. The positive sign for e2qQ can also be explained in terms of a high p-electron density on the tin atom in the direction of the Sn–Fe bond. The i.r. for the products of the insertion reactions are also presented.

Crystal and molecular structure of the orthorhombic modification of NN-dimethyldithiocarbamatotrimethylstannane

The crystal structure of the orthorhombic modification of Me3Sn·S·CS·NMe2 has been determined by single-crystal X-ray diffraction. The unit-cell dimensions are a= 21·61 ± 0·02, b= 14·13 ± 0·03, c= 7·62 ± 0·02 A; Z= 8. Statistical tests based on the generalised ‘R index’ have established the space group to be Pba2 rather than the centrosymmetric Pbam, and have enabled an absolute configuration to be assigned to the particular crystal studied. There are two crystallographically independent molecules in the unit-cell; both have approximately planar SnSC(S)N skeletons with short intramolecular Sn ⋯ S(2) contacts of 3·16 ± 0·03 and 3·33 ± 0·01 A respectively. The other bond lengths are very similar in the two molecules; the mean values are Sn–S(1)= 2·47 ± 0·01, Sn–C = 2·21 ± 0·03, S(1)–C = 1·79 ± 0·02; C–S(2)= 1·71 ± 0·03; C(1)–N = 1·34 ± 0·03, and N–C(5,6)= 1·43 ± 0·03 A.

Metal–metal bonding in co-ordination complexes. Part VII. Crystal structure of dicarbonylcyclopentadienyl(tribromostannyl)iron

The crystal structure of dicarbonyl-π-cyclopentadienyl(tribromostannyl)iron has been determined by single-crystal X-ray methods using the intensities of 1478 spectra measured by counter diffractometry. The crystals are orthorhombic, space group Pbca, a= 12·584(1), b= 13·427(1), c= 15·159(2)A, Z= 8. The structure was solved by symbolic addition methods and refined by block-diagonal least-squares techniques with individual anisotropic thermal parameters to R= 0·04.The molecule contains a short Sn–Fe σ-bond, 2·462(2)A. Fe–Sn–Br and Br–Sn–Br angles lie in the ranges 117·6–118·4 and 98·6–101·6° respectively. Average bond distances are: Sn–Br, 2·501(2); Fe–C(ring), 2·088(2); Fe–C(carbonyl), 1·76(1); C–O, 1·13(1); C–C, 1·394(5)A.Molecular interactions are of normal van der Waals type with no abnormally short inter- or intra-molecular contacts.

Metal–metal bonding in co-ordination complexes. Part VI. Crystal structure of dicarbonylcyclopentadienyl(trichlorostannyl)iron

The crystal and molecular structure of dicarbonyl-π-cyclopentadienyl(trichlorostannyl)iron has been determined by X-ray methods using the intensities of 2561 spectra measured by counter diffractometry. The crystals are triclinic, space group P, a= 11·018(2), b= 8·357(1), c= 6·627(1)A, α= 106·24(1), β= 84·77(1), γ= 96·39(1)°, Z= 2. The structure was determined by the heavy atom method and refined by block-diagonal least-squares techniques with individual anisotropic thermal parameters to R= 0·039.The molecule contains a short Sn–Fe bond, 2·467(2)A, and evidence is presented that this is a σ-bond. The Fe–Sn–Cl and Cl–Sn–Cl angles lie in the ranges 116–121° and 96–100° respectively. The Sn–Cl bond lengths are 2·350(2), 2·358(2), and 2·373(2)A. Mean bond lengths in the (π-C5H5)Fe(CO)2 moiety are : Fe–C(ring), 2·092(3); Fe–C, 1·785(6); C–O, 1·130(8); and C–C, 1·408(5)A. Molecular interactions are of normal van der Waals type and there are no abnormally short intra- or inter-molecular contacts.

Metal–metal bonding in co-ordination complexes. Part VIII. Crystal structure of dicarbonyl-π-cyclopentadienyl[dichloro(phenyl)stannyl]iron

The crystal and molecular structure of dicarbonyl-π-cyclopentadienyl[dichloro(phenyl)stannyl]iron has been determined by single-crystal X-ray diffraction analysis using the intensities of 995 reflections measured by counter diffractometry.Crystals are monoclinic, a= 14·940(2), b= 8·503(1), c= 12·582(2)A, β= 102·98(1)°, Z= 4, space group P21/c. The structure was determined by the heavy-atom method and parameters were refined by block-diagonal least-squares methods to R 0·041. Individual anisotropic thermal parameters were used and no account was taken of hydrogen atoms.The molecule contains a short Sn–Fe σ-bond of length 2·467(2)A. Valence angles around the tin atom are : Fe–Sn–Cl 110·1(1) and 112·9(1), Fe–Sn–C 129·7(3), Cl–Sn–Cl 99·1 (1), and Cl–Sn–C 99·9(4) and 100·5(4)°. Mean bond distances are : Sn–Cl 2·385(3), Sn–C 2·13(1), Fe–C(ring) 2·09(2), Fe–C(carbonyl) 1·75(1), and C–O, 1·16(2)A. There are no abnormally short non-bonded contacts, either inter- or intra-molecular.