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The novel compound bis(1,4,7,10-tetraoxa­cyclo­do­decane)­cadmium(II) decaiodide, [Cd(C8H16O4)2]I10, contains the [Cd(12-crown-4)2]2+ complex cation, triiodide ions and iodine mol­ecules. Two triiodide ions and two iodine mol­ecules form isolated twisted I102- rings. The geometry of the complex cation is as expected, e.g. d(Cd-O) = 2.366 (4) and 2.394 (4) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100008817/jz1406sup1.cif
Contains datablocks [Cd(12k4)2]I10, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100008817/jz1406Isup2.hkl
Contains datablock I

CCDC reference: 150764

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT (Nonius, 1998); data reduction: DENZO (Otwinowski & Minor 1998); program(s) used to solve structure: SHELXS93 (Sheldrick, 1993); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: DIAMOND (Brandenburg, 1998); software used to prepare material for publication: WinGX96 (Farrugia, 1996), PARST95 (Nardelli, 1995), PLATON98 (Spek, 1998), CIFEDIT (Wieczorrek, 1999), ORFFE4 (Busing et al., 1977), LEPAGE (Spek, 1988) maXus (MAC Science Corp. & Nonius, 1998).

Bis-(1,3,5,7-Tetraoxacyclododecan)-cadmium-bis-pentaiodid top
Crystal data top
[Cd(C8H16O4)2]I10Dx = 2.959 Mg m3
Mr = 1733.82Melting point: 416 K
Orthorhombic, FdddMo Kα radiation, λ = 0.71070 Å
Hall symbol: -F 2uv 2vwCell parameters from 22529 reflections
a = 10.914 (1) Åθ = 2.2–25.7°
b = 21.758 (1) ŵ = 8.53 mm1
c = 32.774 (1) ÅT = 293 K
V = 7782.7 (8) Å3Polyeder, metallic red-black
Z = 80.19 × 0.11 × 0.10 mm
F(000) = 6160
Data collection top
κ-CCD Nonius
diffractometer
1853 independent reflections
Radiation source: fine-focus sealed tube1728 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.062
Oscillation Mode scansθmax = 25.7°, θmin = 2.2°
Absorption correction: empirical (using intensity measurements)
(SORTAV; Blessing, 1997).
h = 1313
Tmin = 0.328, Tmax = 0.426k = 2623
22529 measured reflectionsl = 3939
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)] = 0.031Only H-atom displacement parameters refined
wR(F2) = 0.063Calculated w = 1/[σ2(Fo2) + 234P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
1853 reflectionsΔρmax = 1.75 e Å3
83 parametersΔρmin = 1.27 e Å3
0 restraintsExtinction correction: SHELXL93 (Sheldrick, 1993), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.000191 (7)
Special details top

Experimental. Die Strukturlösung mit Direkten Methoden schlug in der hochsymmetrischen Raumgruppe Fddd fehl. Das Strukturmodel konnte in der Raumgruppe P-1 gelöst werden und wurde manuell in die Raumgruppe Fddd transformiert.

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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. 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
I10.1250.34528 (3)0.1250.0463 (2)
I20.17685 (7)0.34470 (2)0.21224 (2)0.0669 (2)
I30.14246 (5)0.18753 (3)0.21079 (2)0.0583 (2)
Cd0.1250.1250.6250.0274 (2)
O10.0585 (4)0.1882 (2)0.56946 (13)0.0406 (10)
C20.1620 (10)0.2149 (4)0.5481 (2)0.069 (2)
H2A0.1335 (10)0.2493 (4)0.5318 (2)0.103 (12)*
H2B0.1958 (10)0.1845 (4)0.5297 (2)0.103 (12)*
C30.2582 (9)0.2362 (4)0.5753 (3)0.071 (3)
H3A0.3301 (9)0.2474 (4)0.5596 (3)0.103 (12)*
H3B0.2305 (9)0.2722 (4)0.5901 (3)0.103 (12)*
O40.2886 (4)0.1885 (2)0.60337 (14)0.0401 (10)
C50.3601 (8)0.2094 (5)0.6380 (3)0.071 (3)
H5A0.4153 (8)0.2416 (5)0.6290 (3)0.103 (12)*
H5B0.4095 (8)0.1755 (5)0.6479 (3)0.103 (12)*
C60.2854 (9)0.2327 (5)0.6713 (3)0.074 (3)
H6A0.3361 (9)0.2396 (5)0.6952 (3)0.103 (12)*
H6B0.2482 (9)0.2714 (5)0.6635 (3)0.103 (12)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.0527 (4)0.0257 (3)0.0604 (4)00.0003 (3)0
I20.1031 (5)0.0432 (3)0.0543 (3)0.0031 (3)0.0093 (3)0.0027 (2)
I30.0519 (3)0.0584 (3)0.0646 (3)0.0102 (2)0.0069 (2)0.0062 (2)
Cd0.0298 (4)0.0213 (4)0.0310 (4)000
O10.050 (3)0.033 (2)0.039 (2)0.003 (2)0.006 (2)0.005 (2)
C20.096 (7)0.065 (5)0.046 (4)0.018 (5)0.003 (4)0.023 (4)
C30.061 (5)0.070 (6)0.083 (6)0.004 (4)0.007 (5)0.042 (5)
O40.038 (2)0.029 (2)0.053 (3)0.004 (2)0.003 (2)0.004 (2)
C50.051 (5)0.078 (6)0.083 (6)0.029 (4)0.002 (4)0.017 (5)
C60.079 (6)0.085 (7)0.058 (5)0.046 (5)0.012 (5)0.002 (4)
Geometric parameters (Å, º) top
I1—I22.9145 (5)Cd—O1ii2.394 (4)
I1—I2i2.9146 (5)Cd—O1iii2.394 (4)
I2—I33.4407 (8)O1—C6iv1.441 (9)
I3—I3ii2.7474 (11)O1—C21.450 (10)
Cd—O4iii2.366 (4)C2—C31.453 (13)
Cd—O4ii2.366 (4)C3—O41.424 (9)
Cd—O4iv2.366 (4)O4—C51.450 (10)
Cd—O42.366 (4)C5—C61.454 (14)
Cd—O12.394 (4)C6—O1iv1.441 (9)
Cd—O1iv2.394 (4)
I2···I3v4.359 (1)O1···O4vi2.742 (6)
I1···Cd6.086 (1)O1···O4vii3.156 (6)
Cd···O12.394 (4)O4···O4viii3.106 (6)
Cd···O42.366 (4)O1···O1vii3.110 (6)
O1···O42.746 (6)
I2—I1—I2i179.50 (3)O4—Cd—O1ii83.1 (2)
I1—I2—I388.26 (2)O1—Cd—O1ii81.0 (2)
I3ii—I3—I2178.12 (3)O1iv—Cd—O1ii144.7 (2)
O4iii—Cd—O4ii108.5 (2)O4iii—Cd—O1iii70.4 (2)
O4iii—Cd—O4iv145.1 (2)O4ii—Cd—O1iii70.3 (2)
O4ii—Cd—O4iv82.1 (2)O4iv—Cd—O1iii83.1 (2)
O4iii—Cd—O482.1 (2)O4—Cd—O1iii142.4 (2)
O4ii—Cd—O4145.1 (2)O1—Cd—O1iii144.7 (2)
O4iv—Cd—O4108.5 (2)O1iv—Cd—O1iii81.0 (2)
O4iii—Cd—O1142.4 (2)O1ii—Cd—O1iii109.8 (2)
O4ii—Cd—O183.1 (2)C6iv—O1—C2112.7 (7)
O4iv—Cd—O170.3 (2)C6iv—O1—Cd116.2 (4)
O4—Cd—O170.4 (2)C2—O1—Cd111.1 (4)
O4iii—Cd—O1iv83.1 (2)O1—C2—C3113.2 (6)
O4ii—Cd—O1iv142.4 (2)O4—C3—C2109.4 (7)
O4iv—Cd—O1iv70.4 (2)C3—O4—C5113.7 (7)
O4—Cd—O1iv70.3 (2)C3—O4—Cd116.3 (5)
O1—Cd—O1iv109.8 (2)C5—O4—Cd110.8 (4)
O4iii—Cd—O1ii70.3 (2)O4—C5—C6113.3 (7)
O4ii—Cd—O1ii70.4 (2)O1iv—C6—C5108.8 (7)
O4iv—Cd—O1ii142.4 (2)
I2i—I1—I2—I36.10 (2)C2—C3—O4—C5165.2 (7)
I1—I2—I3—I3ii103.5 (5)C2—C3—O4—Cd34.8 (9)
O4iii—Cd—O1—C6iv160.3 (6)O4iii—Cd—O4—C3164.3 (6)
O4ii—Cd—O1—C6iv88.2 (6)O4ii—Cd—O4—C353.2 (6)
O4iv—Cd—O1—C6iv4.2 (6)O4iv—Cd—O4—C349.9 (5)
O4—Cd—O1—C6iv114.8 (6)O1—Cd—O4—C310.4 (6)
O1iv—Cd—O1—C6iv55.4 (6)O1iv—Cd—O4—C3110.2 (6)
O1ii—Cd—O1—C6iv159.4 (6)O1ii—Cd—O4—C393.3 (6)
O1iii—Cd—O1—C6iv47.5 (6)O1iii—Cd—O4—C3152.9 (5)
O4iii—Cd—O1—C229.6 (6)O4iii—Cd—O4—C563.8 (5)
O4ii—Cd—O1—C2141.1 (5)O4ii—Cd—O4—C5175.0 (5)
O4iv—Cd—O1—C2134.9 (5)O4iv—Cd—O4—C582.0 (5)
O4—Cd—O1—C215.9 (5)O1—Cd—O4—C5142.2 (5)
O1iv—Cd—O1—C275.3 (5)O1iv—Cd—O4—C521.6 (5)
O1ii—Cd—O1—C269.9 (5)O1ii—Cd—O4—C5134.8 (5)
O1iii—Cd—O1—C2178.2 (5)O1iii—Cd—O4—C521.1 (6)
C6iv—O1—C2—C391.3 (9)C3—O4—C5—C686.1 (9)
Cd—O1—C2—C341.2 (9)Cd—O4—C5—C647.1 (9)
O1—C2—C3—O450.4 (10)O4—C5—C6—O1iv50.2 (11)
Symmetry codes: (i) x+1/4, y, z+1/4; (ii) x+1/4, y+1/4, z; (iii) x, y+1/4, z+5/4; (iv) x+1/4, y, z+5/4; (v) x, y+1/2, z+1/2; (vi) x+3/4, y, z+7/4; (vii) x, y+3/4, z+3/4; (viii) x+3/4, y+3/4, z+1.
 

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