Tin-halide compounds. IV. tert-Butyltrichlorotin(IV)

The mol­ecules of the title compound, [Sn(C₄H₉)Cl₃], adopt an eclipsed conformation with respect to the C and Cl atoms, and possess crystallographic C_s symmetry. The molecular structure and geometric parameters are comparable with those of related organotin trihalides.

Computing details

Data collection: CAD-4 Operations Manual (Enraf-Nonius, 1977); cell refinement: CAD-4 Operations Manual; data reduction: CADSHEL (Kopf & Ruebcke, 1987); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.

tert-Butyltrichlorotin(IV)

Crystal data

[Sn(C4H9)Cl3]	F(000) = 268
Mr = 282.15	Dx = 2.047 Mg m^−3
Monoclinic, P21/m	Mo Kα radiation, λ = 0.71073 Å
a = 7.632 (4) Å	Cell parameters from 25 reflections
b = 10.341 (5) Å	θ = 9.1–20.3°
c = 6.289 (5) Å	µ = 3.58 mm^−1
β = 112.77 (4)°	T = 203 K
V = 457.7 (5) Å^3	Irregular prism, colourless
Z = 2	0.20 × 0.14 × 0.14 mm

Data collection

Enraf-Nonius CAD-4 diffractometer	Rint = 0.026
Radiation source: fine-focus sealed tube	θmax = 25.0°, θmin = 2.9°
Graphite monochromator	h = −9→8
ω/2θ scans	k = 0→12
1715 measured reflections	l = 0→7
836 independent reflections	3 standard reflections every 100 reflections
835 reflections with I > 2σ(I)	intensity decay: 13.5%

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.036	H-atom parameters constrained
wR(F^2) = 0.101	w = 1/[σ^2(Fo^2) + (0.0633P)^2 + 1.6121P] where P = (Fo^2 + 2Fc^2)/3
S = 1.15	(Δ/σ)max = 0.001
836 reflections	Δρmax = 1.82 e Å^−3
45 parameters	Δρmin = −1.06 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.011 (3)

Special details

Experimental. Crystal fixed within a Lindeman capillary

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Sn1	0.51352 (7)	0.2500	0.09210 (8)	0.0313 (3)
Cl1	0.5759 (3)	0.2500	−0.2397 (4)	0.0479 (6)
Cl2	0.6932 (2)	0.07537 (16)	0.2936 (3)	0.0499 (4)
C1	0.2183 (11)	0.2500	0.0534 (13)	0.0350 (17)
C2	0.1873 (9)	0.1294 (7)	0.1722 (12)	0.0480 (15)
H21	0.2075	0.0532	0.0946	0.055 (10)*
H22	0.0583	0.1290	0.1661	0.055 (10)*
H23	0.2761	0.1290	0.3319	0.055 (10)*
C3	0.0961 (12)	0.2500	−0.2039 (15)	0.051 (2)
H31	0.1196	0.3275	−0.2726	0.055 (10)*
H32	−0.0356	0.2500	−0.2265	0.055 (10)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sn1	0.0208 (4)	0.0446 (4)	0.0289 (4)	0.000	0.0100 (2)	0.000
Cl1	0.0405 (12)	0.0757 (15)	0.0334 (10)	0.000	0.0208 (9)	0.000
Cl2	0.0448 (8)	0.0546 (9)	0.0458 (9)	0.0122 (7)	0.0125 (7)	0.0091 (7)
C1	0.026 (4)	0.046 (4)	0.032 (4)	0.000	0.009 (3)	0.000
C2	0.039 (3)	0.054 (4)	0.054 (4)	−0.005 (3)	0.022 (3)	0.002 (3)
C3	0.026 (4)	0.078 (7)	0.038 (5)	0.000	0.002 (4)	0.000

Geometric parameters (Å, º)

Sn1—C1	2.170 (8)	C2—H21	0.9700
Sn1—Cl1	2.313 (3)	C2—H22	0.9700
Sn1—Cl2	2.324 (2)	C2—H23	0.9700
C1—C2	1.519 (8)	C3—H31	0.9600
C1—C3	1.523 (11)	C3—H32	0.9593
C1—Sn1—Cl1	117.8 (2)	C1—C2—H22	109.5
C1—Sn1—Cl2	115.40 (11)	H21—C2—H22	109.5
Cl1—Sn1—Cl2	102.01 (6)	C1—C2—H23	109.5
Cl2^i—Sn1—Cl2	101.97 (10)	H21—C2—H23	109.5
C2—C1—C2^i	110.4 (7)	H22—C2—H23	109.5
C2—C1—C3	112.0 (4)	C1—C3—H31	109.5
C2—C1—Sn1	107.3 (4)	C1—C3—H32	109.5
C3—C1—Sn1	107.6 (5)	H31—C3—H32	107.5
C1—C2—H21	109.5
Cl1—Sn1—C1—C2	120.7 (4)	Cl2—Sn1—C1—C3	−120.67 (10)
Cl1—Sn1—C1—C3	0.00 (4)	Cl2—Sn1—C1—C2^i	118.7 (4)
Cl2—Sn1—C1—C2	0.0 (5)

Symmetry code: (i) x, −y+1/2, z.