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The title compound, [Sn2Te2(C4H9)4(CO3)2O2(C8H10N)4]·4CHCl3 or [(p-Me2NC6H4)2TeOSntBu2CO3]2·4CHCl3, contains an almost planar centrosymmetric inorganic Sn2Te2O8C2 core and hypercoordinated Sn and Te atoms. The structure features four secondary intramolecular Te...O contacts.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804028120/bt6560sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804028120/bt6560Isup2.hkl
Contains datablock I

CCDC reference: 259086

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.054
  • wR factor = 0.111
  • Data-to-parameter ratio = 22.4

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.24 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.62 Ratio PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C2 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for C3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Bergerhoff et al., 1996); software used to prepare material for publication: SHELXL97.

tetra-tert-butyl-di-µ3-carbonato-tetrakis[4-(N,N-dimethylamino)phenyl]di- µ-oxo-ditelluriumditin chloroform tetrasolvate top
Crystal data top
[Sn2Te2(C4H9)4(CO3)2O2(C8H10N)4]·4CHCl3F(000) = 1808
Mr = 1831.20Dx = 1.663 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4050 reflections
a = 11.0573 (8) Åθ = 2.3–25.9°
b = 14.4144 (10) ŵ = 1.95 mm1
c = 23.1203 (17) ÅT = 293 K
β = 96.946 (1)°Rod, colourless
V = 3658.0 (5) Å30.50 × 0.15 × 0.10 mm
Z = 2
Data collection top
Bruker SMART CCD area-detector
diffractometer
8301 independent reflections
Radiation source: fine-focus sealed tube6590 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
φ and ω scansθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1413
Tmin = 0.681, Tmax = 0.823k = 1818
22007 measured reflectionsl = 3015
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.111H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0434P)2 + 5.0552P]
where P = (Fo2 + 2Fc2)/3
8301 reflections(Δ/σ)max < 0.001
370 parametersΔρmax = 1.25 e Å3
0 restraintsΔρmin = 1.30 e Å3
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
C10.7036 (5)0.5654 (3)0.0895 (2)0.0199 (11)
C20.7907 (5)0.7886 (4)0.1500 (3)0.0320 (14)
H20.78810.72150.14330.038*
C30.9552 (5)0.4342 (4)0.8796 (3)0.0425 (17)
H31.04420.43540.88110.051*
C110.5094 (4)0.7106 (3)0.0103 (2)0.0179 (11)
C120.5071 (5)0.8027 (4)0.0282 (2)0.0245 (12)
H120.55620.82180.05590.029*
C130.4328 (5)0.8659 (4)0.0052 (3)0.0261 (12)
H130.43270.92730.01750.031*
C140.3569 (5)0.8393 (4)0.0364 (2)0.0222 (12)
C150.3578 (5)0.7464 (4)0.0532 (3)0.0278 (13)
H150.30810.72670.08050.033*
C160.4329 (5)0.6825 (4)0.0294 (2)0.0224 (11)
H160.43130.62040.04030.027*
C170.3127 (6)0.9998 (4)0.0576 (3)0.0370 (15)
H17A0.25421.03550.07560.056*
H17B0.31101.01830.01760.056*
H17C0.39261.01030.07780.056*
C180.2198 (6)0.8751 (5)0.1086 (3)0.0472 (18)
H18A0.17270.92630.12020.071*
H18B0.27800.85650.14070.071*
H18C0.16660.82400.09690.071*
C210.7548 (4)0.7142 (3)0.0671 (2)0.0179 (10)
C220.7503 (4)0.7443 (3)0.1240 (2)0.0200 (11)
H220.68860.72320.15180.024*
C230.8367 (4)0.8055 (4)0.1402 (2)0.0207 (11)
H230.83200.82470.17880.025*
C240.9316 (5)0.8393 (4)0.0995 (2)0.0215 (11)
C250.9337 (5)0.8077 (4)0.0419 (2)0.0284 (13)
H250.99450.82880.01360.034*
C260.8479 (5)0.7463 (4)0.0264 (3)0.0274 (13)
H260.85240.72600.01200.033*
C271.0166 (5)0.9243 (4)0.1760 (3)0.0334 (14)
H27A1.08100.96770.17970.050*
H27B0.93980.95170.19070.050*
H27C1.02940.86930.19790.050*
C281.1180 (5)0.9275 (5)0.0731 (3)0.0388 (16)
H28A1.16880.97040.09080.058*
H28B1.16460.87350.06040.058*
H28C1.08790.95640.04030.058*
C310.5280 (5)0.5294 (4)0.2189 (2)0.0288 (13)
C320.4532 (7)0.6025 (5)0.1841 (3)0.055 (2)
H32A0.50570.64080.16410.082*
H32B0.41210.64010.20990.082*
H32C0.39410.57300.15620.082*
C330.6245 (6)0.5752 (5)0.2623 (3)0.0446 (17)
H33A0.67120.52820.28440.067*
H33B0.58560.61420.28820.067*
H33C0.67750.61210.24160.067*
C340.4456 (7)0.4686 (6)0.2505 (3)0.058 (2)
H34A0.49360.42250.27270.087*
H34B0.38690.43860.22270.087*
H34C0.40410.50610.27620.087*
C410.7453 (5)0.3367 (4)0.1707 (3)0.0297 (13)
C420.7984 (5)0.3219 (4)0.1141 (3)0.0403 (16)
H42A0.83730.37790.10360.060*
H42B0.73440.30580.08400.060*
H42C0.85720.27260.11890.060*
C430.8445 (5)0.3658 (5)0.2191 (3)0.0388 (16)
H43A0.80920.37490.25460.058*
H43B0.88120.42270.20840.058*
H43C0.90550.31820.22470.058*
C440.6829 (6)0.2481 (5)0.1881 (4)0.054 (2)
H44A0.64970.25810.22410.081*
H44B0.74130.19860.19290.081*
H44C0.61840.23190.15820.081*
Cl10.65667 (18)0.83685 (17)0.11664 (10)0.0737 (7)
Cl20.91632 (18)0.83413 (14)0.12077 (9)0.0571 (5)
Cl30.80836 (18)0.80883 (15)0.22509 (8)0.0569 (5)
Cl40.8961 (2)0.35948 (15)0.82413 (10)0.0673 (6)
Cl50.90017 (19)0.54531 (13)0.86730 (14)0.0842 (9)
Cl60.9171 (2)0.39351 (17)0.94649 (10)0.0719 (6)
N10.2831 (4)0.9030 (3)0.0603 (2)0.0289 (11)
N21.0158 (4)0.9004 (3)0.1155 (2)0.0304 (11)
O10.4606 (3)0.3731 (2)0.12399 (15)0.0222 (8)
O20.7387 (3)0.6207 (2)0.05330 (16)0.0234 (8)
O30.7547 (3)0.5574 (2)0.14209 (16)0.0226 (8)
O40.6094 (3)0.5092 (2)0.07606 (15)0.0196 (8)
Sn10.61146 (3)0.44587 (2)0.157210 (15)0.01782 (10)
Te10.62376 (3)0.61672 (2)0.046718 (15)0.01663 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.022 (3)0.019 (3)0.019 (3)0.002 (2)0.003 (2)0.005 (2)
C20.033 (3)0.028 (3)0.035 (3)0.004 (3)0.003 (3)0.007 (3)
C30.023 (3)0.031 (3)0.074 (5)0.001 (2)0.005 (3)0.001 (3)
C110.018 (2)0.016 (2)0.019 (3)0.0020 (19)0.000 (2)0.001 (2)
C120.025 (3)0.023 (3)0.026 (3)0.003 (2)0.005 (2)0.000 (2)
C130.029 (3)0.018 (3)0.033 (3)0.000 (2)0.007 (3)0.001 (2)
C140.019 (3)0.028 (3)0.018 (3)0.001 (2)0.003 (2)0.005 (2)
C150.030 (3)0.024 (3)0.033 (3)0.006 (2)0.017 (3)0.000 (2)
C160.026 (3)0.019 (3)0.022 (3)0.004 (2)0.002 (2)0.005 (2)
C170.040 (4)0.029 (3)0.044 (4)0.003 (3)0.012 (3)0.005 (3)
C180.049 (4)0.041 (4)0.057 (5)0.009 (3)0.029 (4)0.003 (4)
C210.017 (2)0.018 (2)0.019 (3)0.001 (2)0.002 (2)0.003 (2)
C220.018 (3)0.020 (3)0.021 (3)0.002 (2)0.000 (2)0.001 (2)
C230.021 (3)0.026 (3)0.015 (3)0.002 (2)0.002 (2)0.003 (2)
C240.019 (3)0.019 (3)0.027 (3)0.002 (2)0.001 (2)0.003 (2)
C250.027 (3)0.033 (3)0.022 (3)0.015 (2)0.008 (2)0.003 (3)
C260.029 (3)0.032 (3)0.020 (3)0.007 (2)0.003 (2)0.004 (2)
C270.032 (3)0.034 (3)0.036 (4)0.010 (3)0.010 (3)0.007 (3)
C280.029 (3)0.043 (4)0.041 (4)0.017 (3)0.009 (3)0.006 (3)
C310.031 (3)0.034 (3)0.021 (3)0.008 (2)0.003 (3)0.008 (3)
C320.062 (5)0.059 (5)0.042 (4)0.027 (4)0.000 (4)0.016 (4)
C330.050 (4)0.055 (4)0.028 (4)0.016 (3)0.006 (3)0.019 (3)
C340.065 (5)0.074 (6)0.040 (4)0.023 (4)0.028 (4)0.018 (4)
C410.023 (3)0.031 (3)0.034 (3)0.003 (2)0.002 (3)0.012 (3)
C420.029 (3)0.038 (4)0.053 (4)0.011 (3)0.001 (3)0.000 (3)
C430.029 (3)0.051 (4)0.035 (4)0.008 (3)0.003 (3)0.009 (3)
C440.038 (4)0.038 (4)0.084 (6)0.000 (3)0.001 (4)0.030 (4)
Cl10.0487 (11)0.1032 (17)0.0614 (13)0.0278 (11)0.0247 (10)0.0375 (13)
Cl20.0613 (12)0.0593 (12)0.0555 (12)0.0139 (9)0.0266 (10)0.0098 (10)
Cl30.0637 (12)0.0758 (14)0.0306 (9)0.0045 (10)0.0027 (9)0.0019 (9)
Cl40.0748 (14)0.0679 (14)0.0596 (13)0.0059 (11)0.0102 (11)0.0172 (11)
Cl50.0602 (13)0.0372 (11)0.163 (3)0.0115 (9)0.0436 (15)0.0165 (13)
Cl60.0657 (13)0.0952 (17)0.0532 (13)0.0127 (12)0.0004 (11)0.0003 (12)
N10.030 (3)0.027 (3)0.031 (3)0.003 (2)0.008 (2)0.002 (2)
N20.027 (3)0.035 (3)0.028 (3)0.009 (2)0.004 (2)0.010 (2)
O10.0221 (18)0.028 (2)0.0156 (19)0.0089 (15)0.0024 (15)0.0028 (16)
O20.027 (2)0.024 (2)0.020 (2)0.0050 (16)0.0042 (16)0.0041 (16)
O30.0210 (18)0.028 (2)0.0171 (19)0.0057 (15)0.0022 (15)0.0001 (16)
O40.0219 (18)0.0188 (18)0.0172 (19)0.0016 (14)0.0012 (15)0.0027 (15)
Sn10.01702 (18)0.02152 (19)0.01437 (18)0.00305 (14)0.00044 (14)0.00216 (15)
Te10.01721 (17)0.01580 (16)0.01659 (18)0.00163 (13)0.00086 (13)0.00057 (14)
Geometric parameters (Å, º) top
Sn1—O12.040 (3)C22—C231.384 (7)
Sn1—O32.313 (3)C22—H220.9300
Sn1—O42.085 (3)C23—C241.408 (7)
Sn1—C312.157 (6)C23—H230.9300
Sn1—C412.157 (5)C24—N21.364 (6)
Te1—O1i1.918 (3)C24—C251.405 (7)
Te1—O22.501 (4)C25—C261.377 (7)
Te1—C112.097 (5)C25—H250.9300
Te1—C212.112 (5)C26—H260.9300
C1—O21.252 (6)C27—N21.443 (7)
C1—O31.282 (6)C27—H27A0.9600
C1—O41.326 (6)C27—H27B0.9600
C1—Sn12.615 (5)C27—H27C0.9600
C2—Cl11.731 (6)C28—N21.456 (7)
C2—Cl21.745 (6)C28—H28A0.9600
C2—Cl31.749 (6)C28—H28B0.9600
C2—H20.9800C28—H28C0.9600
C3—Cl51.724 (6)C31—C321.509 (9)
C3—Cl41.740 (7)C31—C341.515 (8)
C3—Cl61.753 (8)C31—C331.524 (8)
C3—H30.9800C32—H32A0.9600
C11—C161.382 (7)C32—H32B0.9600
C11—C121.390 (7)C32—H32C0.9600
C12—C131.376 (7)C33—H33A0.9600
C12—H120.9300C33—H33B0.9600
C13—C141.405 (7)C33—H33C0.9600
C13—H130.9300C34—H34A0.9600
C14—N11.385 (7)C34—H34B0.9600
C14—C151.395 (8)C34—H34C0.9600
C15—C161.397 (7)C41—C421.513 (9)
C15—H150.9300C41—C431.527 (8)
C16—H160.9300C41—C441.528 (8)
C17—N11.437 (7)C42—H42A0.9600
C17—H17A0.9600C42—H42B0.9600
C17—H17B0.9600C42—H42C0.9600
C17—H17C0.9600C43—H43A0.9600
C18—N11.445 (8)C43—H43B0.9600
C18—H18A0.9600C43—H43C0.9600
C18—H18B0.9600C44—H44A0.9600
C18—H18C0.9600C44—H44B0.9600
C21—C221.382 (7)C44—H44C0.9600
C21—C261.387 (7)
C1—O2—Te1116.1 (3)C24—C23—H23119.2
C1—O3—Sn188.5 (3)N2—C24—C25122.1 (5)
C1—O4—Sn197.7 (3)N2—C24—C23121.4 (5)
O1—Sn1—O3147.58 (13)C25—C24—C23116.5 (5)
O1—Sn1—O488.12 (14)C26—C25—C24121.5 (5)
O3—Sn1—O459.50 (13)C26—C25—H25119.3
O1—Sn1—C3198.05 (18)C24—C25—H25119.3
O1—Sn1—C41101.25 (19)C25—C26—C21121.1 (5)
O3—Sn1—C3193.88 (18)C25—C26—H26119.4
O3—Sn1—C4193.35 (18)C21—C26—H26119.4
O4—Sn1—C31113.03 (19)N2—C27—H27A109.5
O4—Sn1—C41112.51 (19)N2—C27—H27B109.5
C31—Sn1—C41130.7 (2)H27A—C27—H27B109.5
O1i—Te1—O2174.14 (13)N2—C27—H27C109.5
O1i—Te1—C1194.36 (18)H27A—C27—H27C109.5
O1i—Te1—C2190.64 (17)H27B—C27—H27C109.5
O2—Te1—C1182.95 (16)N2—C28—H28A109.5
O2—Te1—C2184.54 (16)N2—C28—H28B109.5
C11—Te1—C2197.10 (19)H28A—C28—H28B109.5
Te1i—O1—Sn1126.49 (18)N2—C28—H28C109.5
O2—C1—O3123.7 (5)H28A—C28—H28C109.5
O2—C1—O4122.0 (5)H28B—C28—H28C109.5
O3—C1—O4114.3 (5)C32—C31—C34109.8 (6)
O2—C1—Sn1174.2 (4)C32—C31—C33110.1 (6)
O3—C1—Sn162.1 (3)C34—C31—C33110.3 (5)
O4—C1—Sn152.2 (2)C32—C31—Sn1106.8 (4)
Cl1—C2—Cl2110.8 (4)C34—C31—Sn1109.0 (4)
Cl1—C2—Cl3111.2 (3)C33—C31—Sn1110.8 (4)
Cl2—C2—Cl3108.8 (3)C31—C32—H32A109.5
Cl1—C2—H2108.6C31—C32—H32B109.5
Cl2—C2—H2108.6H32A—C32—H32B109.5
Cl3—C2—H2108.6C31—C32—H32C109.5
Cl5—C3—Cl4111.1 (4)H32A—C32—H32C109.5
Cl5—C3—Cl6109.8 (4)H32B—C32—H32C109.5
Cl4—C3—Cl6109.5 (3)C31—C33—H33A109.5
Cl5—C3—H3108.8C31—C33—H33B109.5
Cl4—C3—H3108.8H33A—C33—H33B109.5
Cl6—C3—H3108.8C31—C33—H33C109.5
C16—C11—C12119.2 (5)H33A—C33—H33C109.5
C16—C11—Te1121.6 (4)H33B—C33—H33C109.5
C12—C11—Te1119.1 (4)C31—C34—H34A109.5
C13—C12—C11120.5 (5)C31—C34—H34B109.5
C13—C12—H12119.8H34A—C34—H34B109.5
C11—C12—H12119.8C31—C34—H34C109.5
C12—C13—C14121.2 (5)H34A—C34—H34C109.5
C12—C13—H13119.4H34B—C34—H34C109.5
C14—C13—H13119.4C42—C41—C43110.7 (5)
N1—C14—C15120.7 (5)C42—C41—C44110.1 (6)
N1—C14—C13121.4 (5)C43—C41—C44110.2 (5)
C15—C14—C13117.9 (5)C42—C41—Sn1108.0 (4)
C14—C15—C16120.6 (5)C43—C41—Sn1109.0 (4)
C14—C15—H15119.7C44—C41—Sn1108.9 (4)
C16—C15—H15119.7C41—C42—H42A109.5
C11—C16—C15120.6 (5)C41—C42—H42B109.5
C11—C16—H16119.7H42A—C42—H42B109.5
C15—C16—H16119.7C41—C42—H42C109.5
N1—C17—H17A109.5H42A—C42—H42C109.5
N1—C17—H17B109.5H42B—C42—H42C109.5
H17A—C17—H17B109.5C41—C43—H43A109.5
N1—C17—H17C109.5C41—C43—H43B109.5
H17A—C17—H17C109.5H43A—C43—H43B109.5
H17B—C17—H17C109.5C41—C43—H43C109.5
N1—C18—H18A109.5H43A—C43—H43C109.5
N1—C18—H18B109.5H43B—C43—H43C109.5
H18A—C18—H18B109.5C41—C44—H44A109.5
N1—C18—H18C109.5C41—C44—H44B109.5
H18A—C18—H18C109.5H44A—C44—H44B109.5
H18B—C18—H18C109.5C41—C44—H44C109.5
C22—C21—C26118.7 (5)H44A—C44—H44C109.5
C22—C21—Te1118.3 (4)H44B—C44—H44C109.5
C26—C21—Te1123.0 (4)C14—N1—C17118.6 (5)
C21—C22—C23120.7 (5)C14—N1—C18119.1 (5)
C21—C22—H22119.6C17—N1—C18115.9 (5)
C23—C22—H22119.6C24—N2—C27120.0 (5)
C22—C23—C24121.6 (5)C24—N2—C28119.4 (5)
C22—C23—H23119.2C27—N2—C28119.6 (5)
Symmetry code: (i) x+1, y+1, z.
 

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