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The title compound, [Sn(C8H9)4], with Sn located at a site of symmetry \overline 4, crystallizes close-packed in the same tetragonal space group (P\overline 421c) as tetra­phenyl­tin. Both mol­ecules may be considered quasi-spherical.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016167/tk6124sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016167/tk6124Isup2.hkl
Contains datablock I

CCDC reference: 221653

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.038
  • wR factor = 0.099
  • Data-to-parameter ratio = 17.8

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

REFLT_03 From the CIF: _diffrn_reflns_theta_max 70.00 From the CIF: _reflns_number_total 1390 Count of symmetry unique reflns 809 Completeness (_total/calc) 171.82% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 581 Fraction of Friedel pairs measured 0.718 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: NRC-2 and NRC-2A (Ahmed et al., 1973); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL96 (Sheldrick, 1996); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL96.

Tetrakis(3,5-dimethylphenyl)tin(IV) top
Crystal data top
[Sn(C8H9)4]Dx = 1.216 Mg m3
Mr = 539.30Melting point: 426-428 K K
Tetragonal, P421cCu Kα radiation, λ = 1.54178 Å
Hall symbol: P -4 2nCell parameters from 25 reflections
a = 13.4000 (19) Åθ = 17.0–20.0°
c = 8.2000 (16) ŵ = 7.00 mm1
V = 1472.4 (4) Å3T = 293 K
Z = 2Needle, colourless
F(000) = 556.00.53 × 0.11 × 0.07 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
1182 reflections with I > 2σ(I)
Radiation source: normal-focus xray tubeRint = 0.071
Graphite monochromatorθmax = 70.0°, θmin = 4.7°
ω scansh = 1616
Absorption correction: integration
(ABSORP in NRCVAX; Gabe et al, 1989)
k = 1616
Tmin = 0.289, Tmax = 0.659l = 99
20587 measured reflections5 standard reflections every 60 min
1390 independent reflections intensity decay: 1.6%
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.038 w = 1/[σ2(Fo2) + (0.0637P)2 + 0.1298P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.099(Δ/σ)max = 0.001
S = 1.13Δρmax = 0.58 e Å3
1390 reflectionsΔρmin = 0.42 e Å3
78 parametersExtinction correction: SHELXL96, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0055 (6)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983), 581 Friedel pairs
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.01 (3)
Special details top

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. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factor_obs 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 (Å2) top
xyzUiso*/Ueq
Sn0.50000.50000.00000.0716 (2)
C10.4281 (3)0.3915 (3)0.1500 (6)0.0727 (10)
C20.4450 (3)0.2895 (3)0.1262 (6)0.0779 (10)
H20.48870.26900.04470.093*
C30.3983 (3)0.2189 (3)0.2215 (6)0.0839 (11)
C40.3314 (4)0.2507 (4)0.3390 (7)0.0922 (14)
H40.29790.20300.40060.111*
C50.3123 (5)0.3499 (4)0.3684 (8)0.0913 (14)
C60.3619 (4)0.4186 (3)0.2702 (7)0.0884 (13)
H60.34960.48620.28660.106*
C70.4217 (6)0.1086 (3)0.1962 (8)0.133 (2)
H7A0.43850.09720.08400.200*
H7B0.36430.06940.22480.200*
H7C0.47700.08990.26410.200*
C80.2410 (5)0.3813 (4)0.4988 (9)0.142 (2)
H8A0.18020.34390.48870.212*
H8B0.22670.45120.48760.212*
H8C0.27010.36910.60380.212*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn0.0624 (2)0.0624 (2)0.0899 (4)0.0000.0000.000
C10.072 (2)0.060 (2)0.086 (3)0.0029 (16)0.006 (2)0.0031 (19)
C20.090 (2)0.062 (2)0.081 (2)0.0042 (17)0.001 (2)0.0015 (19)
C30.102 (3)0.060 (2)0.090 (3)0.003 (2)0.010 (2)0.001 (2)
C40.093 (3)0.074 (3)0.110 (4)0.011 (2)0.002 (3)0.021 (3)
C50.092 (3)0.077 (3)0.105 (4)0.004 (2)0.019 (3)0.013 (3)
C60.095 (3)0.061 (2)0.110 (3)0.010 (2)0.008 (3)0.007 (2)
C70.207 (6)0.058 (2)0.136 (5)0.000 (3)0.006 (5)0.003 (3)
C80.152 (5)0.126 (4)0.147 (5)0.030 (4)0.065 (5)0.026 (4)
Geometric parameters (Å, º) top
Sn—C1i2.134 (5)C4—H40.9300
Sn—C1ii2.134 (5)C5—C61.392 (7)
Sn—C1iii2.134 (5)C5—C81.495 (8)
Sn—C12.134 (5)C6—H60.9300
C1—C61.375 (8)C7—H7A0.9600
C1—C21.400 (5)C7—H7B0.9600
C2—C31.377 (6)C7—H7C0.9600
C2—H20.9300C8—H8A0.9600
C3—C41.383 (6)C8—H8B0.9600
C3—C71.525 (5)C8—H8C0.9600
C4—C51.374 (8)
C1i—Sn—C1ii109.40 (12)C4—C5—C6116.7 (5)
C1i—Sn—C1iii109.40 (12)C4—C5—C8121.1 (5)
C1ii—Sn—C1iii109.6 (2)C6—C5—C8122.2 (5)
C1i—Sn—C1109.6 (2)C1—C6—C5123.2 (4)
C1ii—Sn—C1109.40 (12)C1—C6—H6118.4
C1iii—Sn—C1109.40 (12)C5—C6—H6118.4
C6—C1—C2117.6 (5)C3—C7—H7A109.5
C6—C1—Sn121.7 (3)C3—C7—H7B109.5
C2—C1—Sn120.8 (4)H7A—C7—H7B109.5
C3—C2—C1121.2 (4)C3—C7—H7C109.5
C3—C2—H2119.4H7A—C7—H7C109.5
C1—C2—H2119.4H7B—C7—H7C109.5
C2—C3—C4118.6 (4)C5—C8—H8A109.5
C2—C3—C7119.7 (5)C5—C8—H8B109.5
C4—C3—C7121.8 (5)H8A—C8—H8B109.5
C5—C4—C3122.7 (5)C5—C8—H8C109.5
C5—C4—H4118.6H8A—C8—H8C109.5
C3—C4—H4118.6H8B—C8—H8C109.5
C1i—Sn—C1—C653.4 (4)C1—C2—C3—C7177.7 (5)
C1ii—Sn—C1—C666.5 (3)C2—C3—C4—C52.4 (8)
C1iii—Sn—C1—C6173.4 (4)C7—C3—C4—C5177.2 (6)
C1i—Sn—C1—C2128.2 (4)C3—C4—C5—C61.8 (10)
C1ii—Sn—C1—C2111.9 (5)C3—C4—C5—C8178.7 (6)
C1iii—Sn—C1—C28.2 (4)C2—C1—C6—C50.4 (8)
C6—C1—C2—C31.0 (7)Sn—C1—C6—C5178.9 (5)
Sn—C1—C2—C3179.4 (3)C4—C5—C6—C10.8 (10)
C1—C2—C3—C41.9 (6)C8—C5—C6—C1179.7 (6)
Symmetry codes: (i) x+1, y+1, z; (ii) y, x+1, z; (iii) y+1, x, z.
 

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