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The crystal structure of di-tert-butyl­hydroxido­iodido­tin(IV), [Sn(C4H9)2I(OH)] or tBu2Sn(OH)I, consists of centrosymmetric dimers exhibiting the characteristic structural features of diorganotin(IV)-hydroxide-halides.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S205698902200514X/wm5646sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205698902200514X/wm5646Isup2.hkl
Contains datablock I

CCDC reference: 2172420

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.016
  • wR factor = 0.037
  • Data-to-parameter ratio = 25.9

checkCIF/PLATON results

No syntax errors found



Alert level G PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 1 Report PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ Please Check PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... Check PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 1 Note PLAT933_ALERT_2_G Number of HKL-OMIT Records in Embedded .res File 1 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 4 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 0 ALERT level C = Check. Ensure it is not caused by an omission or oversight 6 ALERT level G = General information/check it is not something unexpected 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS (Sheldrick, 2008); program(s) used to refine structure: SHELXL (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2006) and Mercury (Macrae et al., 2020); software used to prepare material for publication: publCIF (Westrip, 2010).

Di-tert-butylhydroxidoiodidotin(IV) top
Crystal data top
[Sn(C4H9)2I(OH)]F(000) = 712
Mr = 376.82Dx = 2.048 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 8.4903 (4) ÅCell parameters from 9771 reflections
b = 10.8848 (5) Åθ = 2.4–29.2°
c = 13.5107 (6) ŵ = 4.58 mm1
β = 101.881 (2)°T = 100 K
V = 1221.85 (10) Å3Block, yellow
Z = 40.24 × 0.12 × 0.09 mm
Data collection top
Bruker APEXII CCD
diffractometer
2761 reflections with I > 2σ(I)
φ and ω scansRint = 0.064
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
θmax = 28.0°, θmin = 2.6°
Tmin = 0.457, Tmax = 0.715h = 1111
48755 measured reflectionsk = 1413
2950 independent reflectionsl = 1717
Refinement top
Refinement on F2Hydrogen site location: mixed
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.016 w = 1/[σ2(Fo2) + (0.0075P)2 + 1.3137P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.037(Δ/σ)max = 0.003
S = 1.08Δρmax = 0.85 e Å3
2950 reflectionsΔρmin = 0.49 e Å3
114 parametersExtinction correction: SHELXL-2014/7 (Sheldrick 2015, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00139 (11)
Primary atom site location: structure-invariant direct methods
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
I10.31459 (2)0.21150 (2)0.53430 (2)0.01973 (5)
Sn10.06240 (2)0.37120 (2)0.43364 (2)0.01006 (5)
C210.1879 (2)0.44568 (19)0.32082 (15)0.0137 (4)
C220.2375 (3)0.3375 (2)0.26155 (17)0.0193 (5)
H22A0.14090.29560.22470.032 (4)*
H22B0.30270.27980.30860.032 (4)*
H22C0.30040.36790.21350.032 (4)*
C230.3377 (3)0.5141 (2)0.37485 (17)0.0190 (4)
H23A0.39720.54450.32490.023 (4)*
H23B0.40640.45820.42180.023 (4)*
H23C0.30590.58350.41260.023 (4)*
C240.0749 (3)0.5304 (2)0.24902 (16)0.0190 (4)
H24A0.12730.55690.19440.027 (4)*
H24B0.04950.60250.28630.027 (4)*
H24C0.02460.48630.22030.027 (4)*
C110.1328 (3)0.23567 (19)0.40781 (16)0.0153 (4)
C120.2895 (3)0.2973 (2)0.35517 (19)0.0233 (5)
H12A0.27540.33310.29100.029 (4)*
H12B0.31750.36230.39870.029 (4)*
H12C0.37590.23620.34210.029 (4)*
C130.0867 (3)0.1346 (2)0.34001 (18)0.0214 (5)
H13A0.07980.16970.27420.028 (4)*
H13B0.16870.06990.33040.028 (4)*
H13C0.01780.09970.37210.028 (4)*
C140.1500 (3)0.1809 (2)0.50925 (18)0.0236 (5)
H14A0.23510.11850.49790.029 (4)*
H14B0.17810.24610.55260.029 (4)*
H14C0.04800.14310.54230.029 (4)*
O10.09927 (17)0.46366 (13)0.56977 (10)0.0150 (3)
H10.18410.42720.61900.070 (12)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.02092 (9)0.01756 (8)0.01844 (8)0.00750 (5)0.00125 (6)0.00161 (5)
Sn10.01100 (8)0.00881 (8)0.01046 (7)0.00010 (5)0.00239 (5)0.00050 (5)
C210.0164 (10)0.0130 (10)0.0128 (9)0.0014 (8)0.0051 (8)0.0012 (8)
C220.0235 (12)0.0175 (11)0.0188 (11)0.0001 (9)0.0085 (9)0.0039 (9)
C230.0180 (11)0.0196 (11)0.0206 (11)0.0048 (9)0.0067 (9)0.0020 (9)
C240.0236 (11)0.0176 (11)0.0158 (10)0.0020 (9)0.0040 (9)0.0041 (8)
C110.0170 (10)0.0131 (10)0.0171 (10)0.0037 (8)0.0064 (8)0.0040 (8)
C120.0153 (11)0.0226 (12)0.0308 (13)0.0029 (9)0.0018 (9)0.0057 (10)
C130.0223 (12)0.0173 (11)0.0255 (12)0.0036 (9)0.0070 (9)0.0083 (9)
C140.0295 (13)0.0198 (12)0.0250 (12)0.0054 (10)0.0135 (10)0.0012 (9)
O10.0166 (7)0.0147 (7)0.0126 (7)0.0047 (6)0.0004 (6)0.0021 (6)
Geometric parameters (Å, º) top
I1—Sn12.8734 (2)C24—H24C0.9800
Sn1—O12.0631 (1)C11—C121.528 (3)
Sn1—C212.187 (2)C11—C141.529 (3)
Sn1—C112.193 (2)C11—C131.533 (3)
Sn1—O1i2.2564 (1)C12—H12A0.9800
C21—C231.524 (3)C12—H12B0.9800
C21—C241.526 (3)C12—H12C0.9800
C21—C221.531 (3)C13—H13A0.9800
C22—H22A0.9800C13—H13B0.9800
C22—H22B0.9800C13—H13C0.9800
C22—H22C0.9800C14—H14A0.9800
C23—H23A0.9800C14—H14B0.9800
C23—H23B0.9800C14—H14C0.9800
C23—H23C0.9800O1—Sn1i2.2563 (14)
C24—H24A0.9800O1—H10.9600
C24—H24B0.9800
O1—Sn1—C21115.73 (7)C21—C24—H24C109.5
O1—Sn1—C11116.17 (7)H24A—C24—H24C109.5
C21—Sn1—C11126.81 (8)H24B—C24—H24C109.5
O1—Sn1—O1i67.02 (6)C12—C11—C14110.71 (19)
C21—Sn1—O1i94.13 (7)C12—C11—C13109.99 (18)
C11—Sn1—O1i95.51 (7)C14—C11—C13109.84 (19)
O1—Sn1—I184.93 (4)C12—C11—Sn1109.60 (14)
C21—Sn1—I197.57 (5)C14—C11—Sn1109.16 (14)
C11—Sn1—I197.67 (6)C13—C11—Sn1107.47 (14)
O1i—Sn1—I1151.94 (4)C11—C12—H12A109.5
C23—C21—C24111.25 (18)C11—C12—H12B109.5
C23—C21—C22109.50 (17)H12A—C12—H12B109.5
C24—C21—C22109.69 (17)C11—C12—H12C109.5
C23—C21—Sn1109.00 (13)H12A—C12—H12C109.5
C24—C21—Sn1109.55 (13)H12B—C12—H12C109.5
C22—C21—Sn1107.78 (14)C11—C13—H13A109.5
C21—C22—H22A109.5C11—C13—H13B109.5
C21—C22—H22B109.5H13A—C13—H13B109.5
H22A—C22—H22B109.5C11—C13—H13C109.5
C21—C22—H22C109.5H13A—C13—H13C109.5
H22A—C22—H22C109.5H13B—C13—H13C109.5
H22B—C22—H22C109.5C11—C14—H14A109.5
C21—C23—H23A109.5C11—C14—H14B109.5
C21—C23—H23B109.5H14A—C14—H14B109.5
H23A—C23—H23B109.5C11—C14—H14C109.5
C21—C23—H23C109.5H14A—C14—H14C109.5
H23A—C23—H23C109.5H14B—C14—H14C109.5
H23B—C23—H23C109.5Sn1—O1—Sn1i112.98 (6)
C21—C24—H24A109.5Sn1—O1—H1111.7
C21—C24—H24B109.5Sn1i—O1—H1135.3
H24A—C24—H24B109.5
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···I10.962.933.3862 (14)111
 

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