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The structure of the title compound, [SnCl(C10H13)3], (I), was originally determined at room temperature and published without atomic coordinates by Schomburg, Link, Linoh & Tacke [J. Organomet. Chem. (1988), 339, 69-80]. We report here the structural determination at 150 K. The cell dimension shows a contraction from 22.5251 (8) to 22.3858 (4) Å, as expected.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100015067/qa0440sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100015067/qa0440Isup2.hkl
Contains datablock I

CCDC reference: 156195

Comment top

NO COMMENT

Experimental top

The title compound was prepared from the corresponding oxide and HCl. Crystals were obtained by the slow evaporation of a CHCl3 solution [m.p. 389–390 K;. literature value: m.p. 389.5–390.5 K (Zimmer et al., 1966)].

Refinement top

Molecule (I) crystallized in the cubic system; space group I43 d from the systematic absences. H atoms were treated as riding atoms with C—H = 0.95–0.98 Å. Examination of the structure with PLATON (Spek, 2000) showed that there were no solvent-accessible voids in the crystal lattice.

Computing details top

Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).

Chloro-Tris(2-Methyl-2-Phenylpropyl)-Tin top
Crystal data top
[SnCl(C10H13)3]Mo Kα radiation, λ = 0.71073 Å
Mr = 553.75Cell parameters from 2073 reflections
Cubic, I43dθ = 3.4–27.4°
a = 22.3858 (4) ŵ = 1.02 mm1
V = 11218.1 (3) Å3T = 150 K
Z = 16Block, colourless
F(000) = 45760.38 × 0.25 × 0.13 mm
Dx = 1.311 Mg m3
Data collection top
KappaCCD
diffractometer
2073 independent reflections
Radiation source: fine-focus sealed X-ray tube1602 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ϕ scans and ω scans with κ offsetsθmax = 27.4°, θmin = 3.4°
Absorption correction: multi-scan
(SORTAV; lessing, 1995, 1997)
h = 929
Tmin = 0.701, Tmax = 0.883k = 2329
11754 measured reflectionsl = 2426
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.123 w = 1/[σ2(Fo2) + (0.0747P)2 + 4.8319P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.004
2073 reflectionsΔρmax = 0.43 e Å3
99 parametersΔρmin = 0.59 e Å3
0 restraintsAbsolute structure: Flack (1983), 927 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.06 (6)
Crystal data top
[SnCl(C10H13)3]Z = 16
Mr = 553.75Mo Kα radiation
Cubic, I43dµ = 1.02 mm1
a = 22.3858 (4) ÅT = 150 K
V = 11218.1 (3) Å30.38 × 0.25 × 0.13 mm
Data collection top
KappaCCD
diffractometer
2073 independent reflections
Absorption correction: multi-scan
(SORTAV; lessing, 1995, 1997)
1602 reflections with I > 2σ(I)
Tmin = 0.701, Tmax = 0.883Rint = 0.032
11754 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.123Δρmax = 0.43 e Å3
S = 1.04Δρmin = 0.59 e Å3
2073 reflectionsAbsolute structure: Flack (1983), 927 Friedel pairs
99 parametersAbsolute structure parameter: 0.06 (6)
0 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Sn10.402092 (13)0.597908 (13)0.097908 (13)0.0578 (2)
Cl10.34066 (7)0.65934 (7)0.15934 (7)0.1127 (13)
C10.3382 (2)0.5305 (2)0.0735 (3)0.0739 (14)
C20.3405 (3)0.4703 (3)0.1068 (2)0.0796 (17)
C30.3289 (5)0.4824 (5)0.1742 (3)0.147 (5)
C40.2920 (3)0.4299 (4)0.0823 (3)0.100 (3)
C50.4002 (3)0.4399 (2)0.0977 (2)0.0725 (14)
C60.4251 (3)0.4369 (3)0.0412 (3)0.0750 (15)
C70.4779 (3)0.4084 (3)0.0254 (4)0.096 (2)
C80.5078 (5)0.3803 (4)0.0657 (4)0.119 (3)
C90.4916 (5)0.3788 (3)0.1219 (5)0.110 (3)
C100.4365 (6)0.4099 (3)0.1415 (4)0.131 (4)
H1A0.29780.54760.07910.089*
H1B0.34310.52230.03030.089*
H3A0.32180.44440.19480.220*
H3B0.29370.50810.17860.220*
H3C0.36370.50220.19170.220*
H4A0.29830.42390.03940.150*
H4B0.25290.44840.08880.150*
H4C0.29350.39120.10280.150*
H60.40390.45640.01000.090*
H70.49170.40950.01470.115*
H80.54320.36000.05420.143*
H90.51510.35760.15010.132*
H100.42530.41000.18240.157*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.0578 (2)0.0578 (2)0.0578 (2)0.00548 (14)0.00548 (14)0.00548 (14)
Cl10.1127 (13)0.1127 (13)0.1127 (13)0.0326 (10)0.0326 (10)0.0326 (10)
C10.060 (3)0.089 (4)0.072 (3)0.015 (3)0.009 (2)0.007 (3)
C20.094 (4)0.083 (3)0.061 (3)0.037 (3)0.028 (3)0.010 (3)
C30.221 (10)0.139 (7)0.081 (5)0.093 (7)0.091 (6)0.035 (4)
C40.091 (5)0.112 (5)0.097 (5)0.047 (4)0.039 (4)0.032 (4)
C50.105 (4)0.056 (2)0.057 (3)0.025 (3)0.022 (4)0.003 (2)
C60.064 (3)0.077 (4)0.084 (4)0.015 (3)0.002 (3)0.014 (3)
C70.089 (4)0.089 (4)0.109 (5)0.008 (4)0.003 (4)0.007 (4)
C80.164 (9)0.092 (5)0.100 (6)0.040 (6)0.026 (6)0.012 (5)
C90.127 (6)0.053 (3)0.151 (8)0.001 (4)0.070 (6)0.002 (4)
C100.225 (11)0.072 (4)0.095 (5)0.043 (6)0.054 (6)0.010 (4)
Geometric parameters (Å, º) top
Sn1—C12.149 (5)C4—H4B0.9800
Sn1—C1i2.149 (5)C4—H4C0.9800
Sn1—C1ii2.149 (5)C5—C61.385 (9)
Sn1—Cl12.382 (3)C5—C101.439 (11)
C1—C21.541 (8)C6—C71.389 (9)
C1—H1A0.9900C6—H60.9500
C1—H1B0.9900C7—C81.288 (11)
C2—C51.513 (9)C7—H70.9500
C2—C41.517 (9)C8—C91.310 (14)
C2—C31.555 (8)C8—H80.9500
C3—H3A0.9800C9—C101.483 (15)
C3—H3B0.9800C9—H90.9500
C3—H3C0.9800C10—H100.9500
C4—H4A0.9800
C1—Sn1—C1i117.23 (9)C2—C4—H4A109.5
C1—Sn1—C1ii117.24 (8)C2—C4—H4B109.5
C1i—Sn1—C1ii117.24 (8)H4A—C4—H4B109.5
C1—Sn1—Cl199.67 (15)C2—C4—H4C109.5
C1i—Sn1—Cl199.67 (15)H4A—C4—H4C109.5
C1ii—Sn1—Cl199.67 (15)H4B—C4—H4C109.5
C2—C1—Sn1118.0 (4)C6—C5—C10111.8 (7)
C2—C1—H1A107.8C6—C5—C2119.9 (5)
Sn1—C1—H1A107.8C10—C5—C2128.2 (7)
C2—C1—H1B107.8C5—C6—C7126.6 (7)
Sn1—C1—H1B107.8C5—C6—H6116.7
H1A—C1—H1B107.2C7—C6—H6116.7
C5—C2—C4108.4 (5)C8—C7—C6119.3 (9)
C5—C2—C1111.0 (4)C8—C7—H7120.3
C4—C2—C1108.9 (6)C6—C7—H7120.3
C5—C2—C3110.8 (7)C7—C8—C9122.7 (12)
C4—C2—C3109.5 (5)C7—C8—H8118.6
C1—C2—C3108.2 (6)C9—C8—H8118.6
C2—C3—H3A109.5C8—C9—C10120.2 (9)
C2—C3—H3B109.5C8—C9—H9119.9
H3A—C3—H3B109.5C10—C9—H9119.9
C2—C3—H3C109.5C5—C10—C9119.2 (8)
H3A—C3—H3C109.5C5—C10—H10120.4
H3B—C3—H3C109.5C9—C10—H10120.4
C1i—Sn1—C1—C2152.8 (2)C1—C2—C5—C10136.7 (6)
C1ii—Sn1—C1—C25.2 (6)C3—C2—C5—C1016.5 (8)
Cl1—Sn1—C1—C2101.0 (4)C10—C5—C6—C71.1 (9)
Sn1—C1—C2—C560.6 (5)C2—C5—C6—C7176.9 (6)
Sn1—C1—C2—C4179.8 (4)C5—C6—C7—C81.2 (11)
Sn1—C1—C2—C361.3 (7)C6—C7—C8—C91.9 (12)
C4—C2—C5—C673.9 (7)C7—C8—C9—C100.2 (12)
C1—C2—C5—C645.6 (6)C6—C5—C10—C92.7 (8)
C3—C2—C5—C6165.9 (5)C2—C5—C10—C9175.2 (5)
C4—C2—C5—C10103.8 (7)C8—C9—C10—C52.3 (11)
Symmetry codes: (i) z+1/2, x+1, y1/2; (ii) y+1, z+1/2, x+1/2.

Experimental details

Crystal data
Chemical formula[SnCl(C10H13)3]
Mr553.75
Crystal system, space groupCubic, I43d
Temperature (K)150
a (Å)22.3858 (4)
V3)11218.1 (3)
Z16
Radiation typeMo Kα
µ (mm1)1.02
Crystal size (mm)0.38 × 0.25 × 0.13
Data collection
DiffractometerKappaCCD
diffractometer
Absorption correctionMulti-scan
(SORTAV; lessing, 1995, 1997)
Tmin, Tmax0.701, 0.883
No. of measured, independent and
observed [I > 2σ(I)] reflections
11754, 2073, 1602
Rint0.032
(sin θ/λ)max1)0.647
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.123, 1.04
No. of reflections2073
No. of parameters99
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.43, 0.59
Absolute structureFlack (1983), 927 Friedel pairs
Absolute structure parameter0.06 (6)

Computer programs: KappaCCD Server Software (Nonius, 1997), DENZO (Otwinowski & Minor, 1997), DENZO, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).

 

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