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The crystal structure of catena-poly­[[di-n-butyl­tin(IV)]-μ-glutarato], [Sn(C4H9)2(C5H6O4)], is composed of polymeric chains formed by coordination of glutarate, through both ends, to di-n-butyl­tin. The geometry around the hexacoordinated Sn atom is highly distorted octahedral, and may best be described as based on a skew-trapezoidal planar geometry. The symmetry-related glutarate ligands are asymmetrically coordinated to the Sn atoms, with Sn—O distances of 2.138 (2) and 2.483 (2) Å. The Sn—C distance involving the n-butyl group is 2.124 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802008164/ww6019sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802008164/ww6019Isup2.hkl
Contains datablock I

CCDC reference: 189297

Key indicators

  • Single-crystal X-ray study
  • T = 223 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.028
  • wR factor = 0.066
  • Data-to-parameter ratio = 14.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: COLLECT (Hooft, 1998); cell refinement: HKL DENZO (Otwinowski & Minor, 1997); data reduction: SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SAPI91 (Fan, 1991); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[Sn(C4H9)2(C5H6O4)]Dx = 1.555 Mg m3
Mr = 363.02Melting point: 397 K
Orthorhombic, PccnMo Kα radiation, λ = 0.71073 Å
a = 9.9698 (4) ÅCell parameters from 5771 reflections
b = 15.6977 (4) Åθ = 1.0–27.5°
c = 9.9088 (8) ŵ = 1.65 mm1
V = 1550.76 (15) Å3T = 223 K
Z = 4Plate, colourless
F(000) = 7360.27 × 0.24 × 0.09 mm
Data collection top
Nonius KappaCCD
diffractometer
1727 independent reflections
Radiation source: fine-focus sealed tube1462 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.016
ω and φ scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
(SORTAV; Blessing, 1997)
h = 1211
Tmin = 0.664, Tmax = 0.866k = 2020
5771 measured reflectionsl = 1212
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)] = 0.028H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.066 w = 1/[σ2(Fo2) + 3.123P]
where P = (Fo2 + 2Fc2)/3
S = 1.19(Δ/σ)max = 0.001
1727 reflectionsΔρmax = 0.54 e Å3
118 parametersΔρmin = 0.51 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0189 (17)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sn10.25000.25000.07679 (2)0.01940 (15)
O10.1147 (2)0.24921 (14)0.09068 (18)0.0258 (4)
O20.0030 (2)0.23451 (14)0.09756 (19)0.0272 (5)
C10.2433 (3)0.37660 (19)0.1521 (3)0.0271 (6)
H1A0.274 (4)0.372 (3)0.236 (5)0.060 (4)*
H1B0.324 (5)0.405 (3)0.111 (5)0.060 (4)*
C20.1109 (4)0.4230 (2)0.1385 (4)0.0403 (8)
H2A0.052 (5)0.393 (3)0.189 (5)0.060 (4)*
H2B0.086 (5)0.422 (3)0.046 (5)0.060 (4)*
C30.1174 (5)0.5150 (2)0.1880 (4)0.0477 (9)
H3A0.187 (6)0.546 (3)0.144 (5)0.060 (4)*
H3B0.025 (5)0.544 (3)0.168 (4)0.060 (4)*
C40.1416 (8)0.5226 (4)0.3357 (6)0.0765 (18)
H4A0.114 (5)0.578 (3)0.369 (5)0.060 (4)*
H4B0.227 (6)0.511 (3)0.339 (5)0.060 (4)*
H4C0.085 (5)0.477 (3)0.386 (5)0.060 (4)*
C50.0023 (3)0.24117 (17)0.0265 (3)0.0211 (5)
C60.1250 (3)0.2415 (2)0.1081 (3)0.0251 (6)
H6A0.131 (5)0.189 (3)0.153 (4)0.060 (4)*
H6B0.110 (5)0.290 (3)0.174 (5)0.060 (4)*
C70.25000.25000.0242 (4)0.0253 (8)
H7A0.25850.19930.03470.060 (4)*0.50
H7B0.24150.30070.03470.060 (4)*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.01011 (18)0.0300 (2)0.01811 (18)0.00025 (10)0.0000.000
O10.0098 (9)0.0487 (12)0.0189 (9)0.0010 (9)0.0002 (7)0.0008 (9)
O20.0127 (9)0.0495 (13)0.0193 (10)0.0006 (8)0.0007 (7)0.0003 (8)
C10.0221 (14)0.0291 (13)0.0300 (15)0.0004 (12)0.0009 (13)0.0014 (11)
C20.0290 (17)0.0383 (18)0.054 (2)0.0102 (14)0.0091 (16)0.0061 (16)
C30.052 (3)0.0340 (18)0.057 (2)0.0117 (17)0.0078 (19)0.0020 (16)
C40.107 (5)0.057 (3)0.066 (3)0.038 (3)0.018 (3)0.023 (2)
C50.0112 (11)0.0299 (13)0.0223 (12)0.0006 (10)0.0010 (10)0.0009 (10)
C60.0117 (13)0.0464 (17)0.0172 (12)0.0021 (12)0.0008 (10)0.0019 (12)
C70.0101 (16)0.047 (2)0.0189 (17)0.0020 (17)0.0000.000
Geometric parameters (Å, º) top
Sn1—C12.124 (3)C3—C41.489 (7)
Sn1—C1i2.124 (3)C3—H3A0.95 (5)
Sn1—O12.138 (2)C3—H3B1.05 (5)
Sn1—O1i2.138 (2)C4—H4A0.98 (5)
Sn1—O2i2.483 (2)C4—H4B0.87 (5)
Sn1—O22.483 (2)C4—H4C1.04 (5)
O1—C51.295 (3)C5—C61.504 (4)
O2—C51.234 (3)C6—C71.504 (3)
C1—C21.514 (4)C6—H6A0.94 (5)
C1—H1A0.89 (5)C6—H6B1.01 (5)
C1—H1B1.01 (5)C7—C6ii1.504 (3)
C2—C31.526 (5)C7—H7A0.9900
C2—H2A0.90 (5)C7—H7B0.9900
C2—H2B0.95 (5)
C1—Sn1—C1i138.84 (17)H2A—C2—H2B111 (4)
C1—Sn1—O1104.98 (10)C4—C3—C2113.5 (4)
C1i—Sn1—O1106.68 (10)C4—C3—H3A107 (3)
C1—Sn1—O1i106.68 (10)C2—C3—H3A112 (3)
C1i—Sn1—O1i104.98 (10)C4—C3—H3B107 (2)
O1—Sn1—O1i78.20 (10)C2—C3—H3B108 (3)
C1—Sn1—O2i84.85 (10)H3A—C3—H3B109 (4)
C1i—Sn1—O2i91.81 (10)C3—C4—H4A111 (3)
O1—Sn1—O2i133.66 (7)C3—C4—H4B101 (3)
O1i—Sn1—O2i55.83 (7)H4A—C4—H4B117 (5)
C1—Sn1—O291.81 (10)C3—C4—H4C109 (3)
C1i—Sn1—O284.85 (10)H4A—C4—H4C108 (4)
O1—Sn1—O255.83 (7)H4B—C4—H4C111 (4)
O1i—Sn1—O2133.66 (7)O2—C5—O1119.5 (2)
O2i—Sn1—O2170.49 (9)O2—C5—C6122.7 (2)
C5—O1—Sn199.52 (15)O1—C5—C6117.8 (2)
C5—O2—Sn185.11 (16)C7—C6—C5113.7 (2)
C2—C1—Sn1116.5 (2)C7—C6—H6A107 (3)
C2—C1—H1A115 (3)C5—C6—H6A107 (3)
Sn1—C1—H1A104 (3)C7—C6—H6B114 (3)
C2—C1—H1B117 (3)C5—C6—H6B103 (3)
Sn1—C1—H1B104 (3)H6A—C6—H6B111 (4)
H1A—C1—H1B98 (4)C6ii—C7—C6112.9 (3)
C1—C2—C3113.0 (3)C6ii—C7—H7A109.0
C1—C2—H2A106 (3)C6—C7—H7A109.0
C3—C2—H2A110 (3)C6ii—C7—H7B109.0
C1—C2—H2B108 (3)C6—C7—H7B109.0
C3—C2—H2B110 (3)H7A—C7—H7B107.8
C1—Sn1—O1—C580.87 (18)O2i—Sn1—C1—C2166.1 (3)
C1i—Sn1—O1—C572.49 (18)O2—Sn1—C1—C222.9 (3)
O1i—Sn1—O1—C5174.8 (2)Sn1—C1—C2—C3176.8 (3)
O2i—Sn1—O1—C5178.16 (15)C1—C2—C3—C465.8 (6)
O2—Sn1—O1—C50.95 (15)Sn1—O2—C5—O11.6 (2)
C1—Sn1—O2—C5105.94 (18)Sn1—O2—C5—C6177.6 (3)
C1i—Sn1—O2—C5115.17 (18)Sn1—O1—C5—O21.8 (3)
O1—Sn1—O2—C50.99 (15)Sn1—O1—C5—C6177.4 (2)
O1i—Sn1—O2—C59.3 (2)O2—C5—C6—C711.1 (4)
C1i—Sn1—C1—C2107.1 (3)O1—C5—C6—C7168.1 (2)
O1—Sn1—C1—C232.2 (3)C5—C6—C7—C6ii174.6 (3)
O1i—Sn1—C1—C2114.1 (3)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x1/2, y+1/2, z.
 

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