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The structure of [SnMe3O2C(CH2)3CO2SnMe3]n or {[Sn2(CH3)6(C5H6O4)]}n consists of an infinite layer containing penta­coordinate Sn atoms. There are two formula units, A and B, in the asymmetric unit. Glutarate acts as a tetra­dentate bridging ligand, each glutarate being linked to four different Sn atoms, generating two-dimensional sheets. One ligand links the Sn atoms of unit A, the other the Sn atoms of unit B. The sheets are parallel to each other.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807023926/lx2005sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807023926/lx2005Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.031
  • wR factor = 0.062
  • Data-to-parameter ratio = 29.3

checkCIF/PLATON results

No syntax errors found



Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.500 From the CIF: _refine_ls_abs_structure_Flack_su 0.020 PLAT033_ALERT_2_C Flack Parameter Value Deviates 2 * su from zero. 0.50 PLAT141_ALERT_4_C su on a - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio
Alert level G REFLT03_ALERT_4_G 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. From the CIF: _diffrn_reflns_theta_max 30.02 From the CIF: _reflns_number_total 9389 Count of symmetry unique reflns 5523 Completeness (_total/calc) 170.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3866 Fraction of Friedel pairs measured 0.700 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 1997); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1998); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Poly[bis(trimethyltin)-µ-glutarato] top
Crystal data top
[Sn2(CH3)6(C5H6O4)]F(000) = 1776
Mr = 457.68Dx = 1.786 Mg m3
Dm = 1.786 Mg m3
Dm measured by not measured
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 85056 reflections
a = 10.0053 (1) Åθ = 2.9–30.0°
b = 13.1391 (2) ŵ = 2.94 mm1
c = 25.9006 (5) ÅT = 150 K
V = 3404.83 (9) Å3Block, colourless
Z = 80.25 × 0.25 × 0.15 mm
Data collection top
Nonius KappaCCD
diffractometer
9389 independent reflections
Radiation source: fine-focus sealed tube8432 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
φ and ω scansθmax = 30.0°, θmin = 3.1°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
h = 1314
Tmin = 0.502, Tmax = 0.641k = 1818
42835 measured reflectionsl = 3636
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)] = 0.031H-atom parameters constrained
wR(F2) = 0.062 w = 1/[σ2(Fo2) + (0.0178P)2 + 3.5855P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.003
9389 reflectionsΔρmax = 0.72 e Å3
320 parametersΔρmin = 1.11 e Å3
0 restraintsAbsolute structure: Flack (1983), 3866 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.50 (2)
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. 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 (Å2) top
xyzUiso*/Ueq
Sn10.06139 (3)0.72411 (2)0.975517 (9)0.02341 (6)
Sn20.59702 (3)0.289237 (19)0.983204 (10)0.02409 (6)
Sn30.59362 (3)0.67537 (2)0.719223 (10)0.02360 (6)
Sn40.09138 (3)0.23593 (2)0.732318 (9)0.02403 (6)
O10.0970 (3)0.6309 (2)0.93905 (10)0.0295 (6)
O20.2481 (3)0.6922 (2)0.99309 (11)0.0312 (7)
O30.4428 (3)0.3626 (2)0.93539 (11)0.0294 (6)
O40.2814 (3)0.2724 (2)0.97135 (11)0.0317 (7)
O50.4318 (3)0.5865 (2)0.68381 (10)0.0287 (6)
O60.2816 (3)0.6535 (2)0.73578 (11)0.0301 (7)
O70.0698 (2)0.3250 (2)0.69527 (10)0.0283 (6)
O80.2170 (3)0.2602 (2)0.74952 (11)0.0321 (7)
C10.1909 (4)0.6676 (3)0.91751 (15)0.0294 (9)
H1A0.28300.68760.92540.044*
H1B0.16490.69580.88400.044*
H1C0.18480.59320.91630.044*
C20.0341 (4)0.8660 (3)0.96132 (17)0.0329 (10)
H2A0.03380.91870.95570.049*
H2B0.08940.88440.99110.049*
H2C0.09060.86040.93060.049*
C30.0487 (5)0.6488 (4)1.04777 (16)0.0367 (10)
H3A0.01810.59431.04570.055*
H3B0.02250.69761.07450.055*
H3C0.13600.61951.05650.055*
C40.2169 (4)0.6386 (3)0.95539 (15)0.0248 (8)
C50.3242 (4)0.5817 (3)0.92572 (17)0.0294 (9)
H5A0.37860.63200.90650.035*
H5B0.38400.54790.95090.035*
C60.2744 (4)0.5015 (3)0.88754 (15)0.0296 (9)
H6A0.34920.48190.86460.036*
H6B0.20380.53210.86570.036*
C70.2187 (4)0.4057 (3)0.91298 (17)0.0299 (9)
H7A0.17800.36240.88590.036*
H7B0.14660.42580.93710.036*
C80.3197 (4)0.3432 (3)0.94217 (15)0.0240 (8)
C90.7383 (5)0.3863 (4)0.9466 (2)0.0519 (15)
H9A0.77950.43090.97240.078*
H9B0.80770.34490.93000.078*
H9C0.69300.42770.92040.078*
C100.5126 (4)0.3371 (4)1.05443 (16)0.0352 (10)
H10A0.49750.27771.07660.053*
H10B0.57400.38431.07170.053*
H10C0.42730.37151.04790.053*
C110.5668 (5)0.1406 (3)0.95362 (17)0.0386 (11)
H11A0.49650.10660.97350.058*
H11B0.53990.14490.91730.058*
H11C0.65000.10170.95640.058*
C120.7259 (4)0.6130 (4)0.66366 (18)0.0392 (11)
H12A0.76860.66820.64430.059*
H12B0.79450.57240.68120.059*
H12C0.67560.56940.63980.059*
C130.5747 (5)0.6040 (3)0.79220 (16)0.0367 (10)
H13A0.51740.64550.81450.055*
H13B0.53480.53650.78780.055*
H13C0.66320.59710.80800.055*
C140.5049 (4)0.8173 (3)0.70136 (17)0.0334 (10)
H14A0.57480.86900.69740.050*
H14B0.45440.81150.66910.050*
H14C0.44440.83730.72930.050*
C150.3111 (4)0.5984 (3)0.69849 (15)0.0258 (8)
C160.2056 (4)0.5424 (3)0.66806 (15)0.0243 (8)
H16A0.13090.52490.69150.029*
H16B0.16990.58870.64120.029*
C170.2550 (4)0.4449 (3)0.64197 (15)0.0260 (8)
H17A0.33060.46180.61880.031*
H17B0.18220.41660.62040.031*
C180.3001 (4)0.3644 (3)0.68042 (16)0.0274 (9)
H18A0.36280.39640.70510.033*
H18B0.35010.31120.66150.033*
C190.1890 (4)0.3135 (3)0.71078 (16)0.0266 (8)
C200.0726 (5)0.3066 (3)0.80561 (15)0.0373 (10)
H20A0.16130.32580.81830.056*
H20B0.03090.25910.82990.056*
H20C0.01680.36760.80240.056*
C210.0050 (4)0.0928 (3)0.71434 (18)0.0351 (10)
H21A0.02770.09360.67870.053*
H21B0.06970.07940.73790.053*
H21C0.07250.03920.71820.053*
C220.2247 (4)0.2995 (4)0.67762 (17)0.0418 (12)
H22A0.20550.37230.67360.063*
H22B0.21330.26510.64430.063*
H22C0.31680.29070.68960.063*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sn10.01866 (13)0.02398 (14)0.02758 (12)0.00066 (10)0.00109 (9)0.00234 (11)
Sn20.01943 (12)0.02271 (14)0.03013 (12)0.00074 (11)0.00154 (10)0.00362 (10)
Sn30.02012 (13)0.02231 (14)0.02835 (12)0.00194 (11)0.00207 (11)0.00274 (10)
Sn40.02028 (13)0.02494 (14)0.02687 (11)0.00013 (11)0.00011 (10)0.00457 (10)
O10.0205 (13)0.0310 (15)0.0369 (14)0.0011 (13)0.0022 (13)0.0080 (12)
O20.0231 (14)0.0310 (16)0.0394 (16)0.0004 (13)0.0004 (12)0.0098 (13)
O30.0195 (14)0.0338 (16)0.0348 (14)0.0023 (12)0.0007 (12)0.0087 (12)
O40.0211 (14)0.0300 (16)0.0441 (17)0.0002 (12)0.0033 (12)0.0087 (14)
O50.0190 (15)0.0320 (15)0.0352 (15)0.0040 (12)0.0036 (12)0.0092 (12)
O60.0203 (14)0.0346 (17)0.0356 (15)0.0006 (12)0.0006 (12)0.0119 (14)
O70.0185 (14)0.0302 (15)0.0362 (14)0.0031 (12)0.0009 (11)0.0089 (12)
O80.0262 (14)0.0301 (16)0.0399 (15)0.0055 (13)0.0008 (12)0.0106 (13)
C10.027 (2)0.031 (2)0.0304 (19)0.0008 (18)0.0066 (16)0.0034 (18)
C20.031 (2)0.023 (2)0.045 (2)0.0016 (18)0.0038 (19)0.0001 (18)
C30.035 (2)0.038 (3)0.038 (2)0.007 (2)0.0016 (19)0.0094 (19)
C40.0194 (19)0.023 (2)0.032 (2)0.0025 (16)0.0051 (16)0.0009 (16)
C50.023 (2)0.026 (2)0.039 (2)0.0062 (17)0.0050 (17)0.0001 (18)
C60.032 (2)0.033 (2)0.0234 (19)0.0093 (19)0.0016 (17)0.0016 (16)
C70.022 (2)0.030 (2)0.038 (2)0.0033 (18)0.0061 (17)0.0033 (18)
C80.0206 (19)0.023 (2)0.0287 (19)0.0004 (16)0.0011 (15)0.0024 (16)
C90.028 (2)0.063 (4)0.064 (3)0.004 (2)0.003 (2)0.031 (3)
C100.035 (2)0.037 (3)0.034 (2)0.009 (2)0.0037 (18)0.0080 (19)
C110.043 (3)0.030 (2)0.043 (2)0.009 (2)0.000 (2)0.0084 (19)
C120.029 (2)0.047 (3)0.042 (3)0.002 (2)0.009 (2)0.015 (2)
C130.040 (3)0.031 (2)0.038 (2)0.007 (2)0.002 (2)0.0102 (18)
C140.036 (2)0.027 (2)0.038 (2)0.0023 (19)0.0023 (18)0.0035 (19)
C150.024 (2)0.025 (2)0.0284 (19)0.0022 (17)0.0018 (16)0.0015 (16)
C160.0220 (19)0.024 (2)0.0266 (18)0.0023 (16)0.0028 (15)0.0008 (16)
C170.024 (2)0.029 (2)0.0252 (18)0.0030 (17)0.0035 (16)0.0019 (16)
C180.023 (2)0.028 (2)0.032 (2)0.0001 (17)0.0008 (16)0.0019 (17)
C190.024 (2)0.020 (2)0.035 (2)0.0012 (16)0.0036 (16)0.0006 (17)
C200.044 (3)0.036 (2)0.031 (2)0.006 (2)0.0033 (19)0.0022 (17)
C210.032 (2)0.032 (2)0.041 (2)0.0043 (19)0.0093 (19)0.003 (2)
C220.032 (2)0.054 (3)0.040 (2)0.002 (2)0.0043 (19)0.020 (2)
Geometric parameters (Å, º) top
Sn1—O12.214 (3)C6—C71.526 (6)
Sn1—O2i2.346 (3)C6—H6A0.9900
Sn2—O32.201 (3)C6—H6B0.9900
Sn2—O4ii2.333 (3)C7—C81.506 (5)
Sn3—O52.197 (3)C7—H7A0.9900
Sn3—O8iii2.343 (3)C7—H7B0.9900
Sn4—O72.211 (3)C9—H9A0.9800
O1—C41.276 (5)C9—H9B0.9800
O2—C41.244 (5)C9—H9C0.9800
O3—C81.270 (5)C10—H10A0.9800
O4—C81.258 (5)C10—H10B0.9800
O5—C151.276 (5)C10—H10C0.9800
O6—C151.243 (5)C11—H11A0.9800
O7—C191.268 (5)C11—H11B0.9800
O8—C191.255 (5)C11—H11C0.9800
Sn1—C12.119 (4)C12—H12A0.9800
Sn1—C32.121 (4)C12—H12B0.9800
Sn1—C22.127 (4)C12—H12C0.9800
Sn2—C112.119 (4)C13—H13A0.9800
Sn2—C102.124 (4)C13—H13B0.9800
Sn2—C92.127 (5)C13—H13C0.9800
Sn3—C142.117 (4)C14—H14A0.9800
Sn3—C132.118 (4)C14—H14B0.9800
Sn3—C122.120 (4)C14—H14C0.9800
Sn3—O52.197 (3)C15—C161.509 (5)
Sn4—C222.118 (4)C16—C171.531 (5)
Sn4—C212.122 (4)C16—H16A0.9900
Sn4—C202.122 (4)C16—H16B0.9900
Sn4—O6iv2.340 (3)C17—C181.521 (5)
O4—Sn2v2.333 (3)C17—H17A0.9900
O6—Sn4vi2.340 (3)C17—H17B0.9900
O8—Sn3vii2.343 (3)C18—C191.517 (5)
C1—H1A0.9800C18—H18A0.9900
C1—H1B0.9800C18—H18B0.9900
C1—H1C0.9800C20—H20A0.9800
C2—H2A0.9800C20—H20B0.9800
C2—H2B0.9800C20—H20C0.9800
C2—H2C0.9800C21—H21A0.9800
C3—H3A0.9800C21—H21B0.9800
C3—H3B0.9800C21—H21C0.9800
C3—H3C0.9800C22—H22A0.9800
C4—C51.518 (5)C22—H22B0.9800
C5—C61.529 (6)C22—H22C0.9800
C5—H5A0.9900O2—Sn1viii2.346 (3)
C5—H5B0.9900
C1—Sn1—C2117.35 (17)C8—C7—H7B108.5
C1—Sn1—C3119.91 (18)C6—C7—H7B108.5
C3—Sn1—C2122.34 (18)H7A—C7—H7B107.5
C10—Sn2—C9118.3 (2)O4—C8—O3121.8 (4)
C11—Sn2—C10122.02 (19)O4—C8—C7120.0 (3)
C11—Sn2—C9119.1 (2)O3—C8—C7118.2 (4)
C13—Sn3—C12119.36 (19)Sn2—C9—H9A109.5
C14—Sn3—C13123.19 (18)Sn2—C9—H9B109.5
C14—Sn3—C12117.01 (19)H9A—C9—H9B109.5
C20—Sn4—C21123.25 (18)Sn2—C9—H9C109.5
C22—Sn4—C20118.79 (19)H9A—C9—H9C109.5
C22—Sn4—C21117.4 (2)H9B—C9—H9C109.5
C1—Sn1—O186.64 (13)Sn2—C10—H10A109.5
C1—Sn1—O2i85.01 (13)Sn2—C10—H10B109.5
C2—Sn1—O195.15 (14)H10A—C10—H10B109.5
C2—Sn1—O2i90.80 (14)Sn2—C10—H10C109.5
C3—Sn1—O194.33 (14)H10A—C10—H10C109.5
C3—Sn1—O2i87.79 (15)H10B—C10—H10C109.5
C9—Sn2—O387.29 (15)Sn2—C11—H11A109.5
C9—Sn2—O4ii84.68 (15)Sn2—C11—H11B109.5
C10—Sn2—O394.60 (14)H11A—C11—H11B109.5
C10—Sn2—O4ii88.79 (14)Sn2—C11—H11C109.5
C11—Sn2—O395.74 (15)H11A—C11—H11C109.5
C11—Sn2—O4ii88.60 (14)H11B—C11—H11C109.5
C12—Sn3—O588.33 (14)Sn3—C12—H12A109.5
C12—Sn3—O8iii85.05 (14)Sn3—C12—H12B109.5
C13—Sn3—O594.11 (14)H12A—C12—H12B109.5
C13—Sn3—O8iii88.54 (14)Sn3—C12—H12C109.5
C14—Sn3—O593.89 (14)H12A—C12—H12C109.5
C14—Sn3—O8iii89.75 (14)H12B—C12—H12C109.5
C20—Sn4—O6iv87.64 (14)Sn3—C13—H13A109.5
C21—Sn4—O6iv89.90 (14)Sn3—C13—H13B109.5
C20—Sn4—O795.28 (14)H13A—C13—H13B109.5
C21—Sn4—O794.41 (14)Sn3—C13—H13C109.5
C22—Sn4—O6iv84.66 (14)H13A—C13—H13C109.5
C22—Sn4—O787.70 (14)H13B—C13—H13C109.5
O1—Sn1—O2i171.32 (10)Sn3—C14—H14A109.5
O3—Sn2—O4ii171.96 (10)Sn3—C14—H14B109.5
O5—Sn3—O8iii173.34 (10)H14A—C14—H14B109.5
O7—Sn4—O6iv172.31 (10)Sn3—C14—H14C109.5
C4—O1—Sn1119.2 (2)H14A—C14—H14C109.5
C4—O2—Sn1viii137.8 (3)H14B—C14—H14C109.5
C8—O3—Sn2120.9 (3)O6—C15—O5121.9 (4)
C8—O4—Sn2v143.2 (3)O6—C15—C16121.6 (3)
C15—O5—Sn3120.6 (2)O5—C15—C16116.6 (3)
C15—O6—Sn4vi137.5 (3)C15—C16—C17114.4 (3)
C19—O7—Sn4119.0 (2)C15—C16—H16A108.7
C19—O8—Sn3vii136.2 (3)C17—C16—H16A108.7
Sn1—C1—H1A109.5C15—C16—H16B108.7
Sn1—C1—H1B109.5C17—C16—H16B108.7
H1A—C1—H1B109.5H16A—C16—H16B107.6
Sn1—C1—H1C109.5C18—C17—C16112.9 (3)
H1A—C1—H1C109.5C18—C17—H17A109.0
H1B—C1—H1C109.5C16—C17—H17A109.0
Sn1—C2—H2A109.5C18—C17—H17B109.0
Sn1—C2—H2B109.5C16—C17—H17B109.0
H2A—C2—H2B109.5H17A—C17—H17B107.8
Sn1—C2—H2C109.5C19—C18—C17115.4 (3)
H2A—C2—H2C109.5C19—C18—H18A108.4
H2B—C2—H2C109.5C17—C18—H18A108.4
Sn1—C3—H3A109.5C19—C18—H18B108.4
Sn1—C3—H3B109.5C17—C18—H18B108.4
H3A—C3—H3B109.5H18A—C18—H18B107.5
Sn1—C3—H3C109.5O8—C19—O7121.9 (4)
H3A—C3—H3C109.5O8—C19—C18119.8 (3)
H3B—C3—H3C109.5O7—C19—C18118.2 (3)
O2—C4—O1122.7 (4)Sn4—C20—H20A109.5
O2—C4—C5119.9 (4)Sn4—C20—H20B109.5
O1—C4—C5117.3 (3)H20A—C20—H20B109.5
C4—C5—C6115.9 (3)Sn4—C20—H20C109.5
C4—C5—H5A108.3H20A—C20—H20C109.5
C6—C5—H5A108.3H20B—C20—H20C109.5
C4—C5—H5B108.3Sn4—C21—H21A109.5
C6—C5—H5B108.3Sn4—C21—H21B109.5
H5A—C5—H5B107.4H21A—C21—H21B109.5
C7—C6—C5114.1 (3)Sn4—C21—H21C109.5
C7—C6—H6A108.7H21A—C21—H21C109.5
C5—C6—H6A108.7H21B—C21—H21C109.5
C7—C6—H6B108.7Sn4—C22—H22A109.5
C5—C6—H6B108.7Sn4—C22—H22B109.5
H6A—C6—H6B107.6H22A—C22—H22B109.5
C8—C7—C6114.9 (3)Sn4—C22—H22C109.5
C8—C7—H7A108.5H22A—C22—H22C109.5
C6—C7—H7A108.5H22B—C22—H22C109.5
Symmetry codes: (i) x+1/2, y+3/2, z+2; (ii) x1/2, y+1/2, z+2; (iii) x1, y+1/2, z+3/2; (iv) x, y1/2, z+3/2; (v) x+1/2, y+1/2, z+2; (vi) x, y+1/2, z+3/2; (vii) x1, y1/2, z+3/2; (viii) x1/2, y+3/2, z+2.
 

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