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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
CCDC reference: 150764
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]I10 | Dx = 2.959 Mg m−3 |
Mr = 1733.82 | Melting point: 416 K |
Orthorhombic, Fddd | Mo Kα radiation, λ = 0.71070 Å |
Hall symbol: -F 2uv 2vw | Cell parameters from 22529 reflections |
a = 10.914 (1) Å | θ = 2.2–25.7° |
b = 21.758 (1) Å | µ = 8.53 mm−1 |
c = 32.774 (1) Å | T = 293 K |
V = 7782.7 (8) Å3 | Polyeder, metallic red-black |
Z = 8 | 0.19 × 0.11 × 0.10 mm |
F(000) = 6160 | |
Data collection top
κ-CCD Nonius diffractometer | 1853 independent reflections |
Radiation source: fine-focus sealed tube | 1728 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
Oscillation Mode scans | θmax = 25.7°, θmin = 2.2° |
Absorption correction: empirical (using intensity measurements) (SORTAV; Blessing, 1997). | h = −13→13 |
Tmin = 0.328, Tmax = 0.426 | k = −26→23 |
22529 measured reflections | l = −39→39 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.031 | Only H-atom displacement parameters refined |
wR(F2) = 0.063 | Calculated w = 1/[σ2(Fo2) + 234P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max = 0.001 |
1853 reflections | Δρmax = 1.75 e Å−3 |
83 parameters | Δρmin = −1.27 e Å−3 |
0 restraints | Extinction correction: SHELXL93 (Sheldrick, 1993), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction 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 | x | y | z | Uiso*/Ueq | |
I1 | 0.125 | 0.34528 (3) | 0.125 | 0.0463 (2) | |
I2 | 0.17685 (7) | 0.34470 (2) | 0.21224 (2) | 0.0669 (2) | |
I3 | 0.14246 (5) | 0.18753 (3) | 0.21079 (2) | 0.0583 (2) | |
Cd | 0.125 | 0.125 | 0.625 | 0.0274 (2) | |
O1 | 0.0585 (4) | 0.1882 (2) | 0.56946 (13) | 0.0406 (10) | |
C2 | 0.1620 (10) | 0.2149 (4) | 0.5481 (2) | 0.069 (2) | |
H2A | 0.1335 (10) | 0.2493 (4) | 0.5318 (2) | 0.103 (12)* | |
H2B | 0.1958 (10) | 0.1845 (4) | 0.5297 (2) | 0.103 (12)* | |
C3 | 0.2582 (9) | 0.2362 (4) | 0.5753 (3) | 0.071 (3) | |
H3A | 0.3301 (9) | 0.2474 (4) | 0.5596 (3) | 0.103 (12)* | |
H3B | 0.2305 (9) | 0.2722 (4) | 0.5901 (3) | 0.103 (12)* | |
O4 | 0.2886 (4) | 0.1885 (2) | 0.60337 (14) | 0.0401 (10) | |
C5 | 0.3601 (8) | 0.2094 (5) | 0.6380 (3) | 0.071 (3) | |
H5A | 0.4153 (8) | 0.2416 (5) | 0.6290 (3) | 0.103 (12)* | |
H5B | 0.4095 (8) | 0.1755 (5) | 0.6479 (3) | 0.103 (12)* | |
C6 | 0.2854 (9) | 0.2327 (5) | 0.6713 (3) | 0.074 (3) | |
H6A | 0.3361 (9) | 0.2396 (5) | 0.6952 (3) | 0.103 (12)* | |
H6B | 0.2482 (9) | 0.2714 (5) | 0.6635 (3) | 0.103 (12)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.0527 (4) | 0.0257 (3) | 0.0604 (4) | 0 | −0.0003 (3) | 0 |
I2 | 0.1031 (5) | 0.0432 (3) | 0.0543 (3) | −0.0031 (3) | −0.0093 (3) | 0.0027 (2) |
I3 | 0.0519 (3) | 0.0584 (3) | 0.0646 (3) | −0.0102 (2) | −0.0069 (2) | 0.0062 (2) |
Cd | 0.0298 (4) | 0.0213 (4) | 0.0310 (4) | 0 | 0 | 0 |
O1 | 0.050 (3) | 0.033 (2) | 0.039 (2) | 0.003 (2) | −0.006 (2) | 0.005 (2) |
C2 | 0.096 (7) | 0.065 (5) | 0.046 (4) | −0.018 (5) | −0.003 (4) | 0.023 (4) |
C3 | 0.061 (5) | 0.070 (6) | 0.083 (6) | −0.004 (4) | 0.007 (5) | 0.042 (5) |
O4 | 0.038 (2) | 0.029 (2) | 0.053 (3) | −0.004 (2) | 0.003 (2) | 0.004 (2) |
C5 | 0.051 (5) | 0.078 (6) | 0.083 (6) | −0.029 (4) | −0.002 (4) | −0.017 (5) |
C6 | 0.079 (6) | 0.085 (7) | 0.058 (5) | −0.046 (5) | −0.012 (5) | −0.002 (4) |
Geometric parameters (Å, º) top
I1—I2 | 2.9145 (5) | Cd—O1ii | 2.394 (4) |
I1—I2i | 2.9146 (5) | Cd—O1iii | 2.394 (4) |
I2—I3 | 3.4407 (8) | O1—C6iv | 1.441 (9) |
I3—I3ii | 2.7474 (11) | O1—C2 | 1.450 (10) |
Cd—O4iii | 2.366 (4) | C2—C3 | 1.453 (13) |
Cd—O4ii | 2.366 (4) | C3—O4 | 1.424 (9) |
Cd—O4iv | 2.366 (4) | O4—C5 | 1.450 (10) |
Cd—O4 | 2.366 (4) | C5—C6 | 1.454 (14) |
Cd—O1 | 2.394 (4) | C6—O1iv | 1.441 (9) |
Cd—O1iv | 2.394 (4) | | |
| | | |
I2···I3v | 4.359 (1) | O1···O4vi | 2.742 (6) |
I1···Cd | 6.086 (1) | O1···O4vii | 3.156 (6) |
Cd···O1 | 2.394 (4) | O4···O4viii | 3.106 (6) |
Cd···O4 | 2.366 (4) | O1···O1vii | 3.110 (6) |
O1···O4 | 2.746 (6) | | |
| | | |
I2—I1—I2i | 179.50 (3) | O4—Cd—O1ii | 83.1 (2) |
I1—I2—I3 | 88.26 (2) | O1—Cd—O1ii | 81.0 (2) |
I3ii—I3—I2 | 178.12 (3) | O1iv—Cd—O1ii | 144.7 (2) |
O4iii—Cd—O4ii | 108.5 (2) | O4iii—Cd—O1iii | 70.4 (2) |
O4iii—Cd—O4iv | 145.1 (2) | O4ii—Cd—O1iii | 70.3 (2) |
O4ii—Cd—O4iv | 82.1 (2) | O4iv—Cd—O1iii | 83.1 (2) |
O4iii—Cd—O4 | 82.1 (2) | O4—Cd—O1iii | 142.4 (2) |
O4ii—Cd—O4 | 145.1 (2) | O1—Cd—O1iii | 144.7 (2) |
O4iv—Cd—O4 | 108.5 (2) | O1iv—Cd—O1iii | 81.0 (2) |
O4iii—Cd—O1 | 142.4 (2) | O1ii—Cd—O1iii | 109.8 (2) |
O4ii—Cd—O1 | 83.1 (2) | C6iv—O1—C2 | 112.7 (7) |
O4iv—Cd—O1 | 70.3 (2) | C6iv—O1—Cd | 116.2 (4) |
O4—Cd—O1 | 70.4 (2) | C2—O1—Cd | 111.1 (4) |
O4iii—Cd—O1iv | 83.1 (2) | O1—C2—C3 | 113.2 (6) |
O4ii—Cd—O1iv | 142.4 (2) | O4—C3—C2 | 109.4 (7) |
O4iv—Cd—O1iv | 70.4 (2) | C3—O4—C5 | 113.7 (7) |
O4—Cd—O1iv | 70.3 (2) | C3—O4—Cd | 116.3 (5) |
O1—Cd—O1iv | 109.8 (2) | C5—O4—Cd | 110.8 (4) |
O4iii—Cd—O1ii | 70.3 (2) | O4—C5—C6 | 113.3 (7) |
O4ii—Cd—O1ii | 70.4 (2) | O1iv—C6—C5 | 108.8 (7) |
O4iv—Cd—O1ii | 142.4 (2) | | |
| | | |
I2i—I1—I2—I3 | −6.10 (2) | C2—C3—O4—C5 | −165.2 (7) |
I1—I2—I3—I3ii | −103.5 (5) | C2—C3—O4—Cd | −34.8 (9) |
O4iii—Cd—O1—C6iv | −160.3 (6) | O4iii—Cd—O4—C3 | 164.3 (6) |
O4ii—Cd—O1—C6iv | 88.2 (6) | O4ii—Cd—O4—C3 | 53.2 (6) |
O4iv—Cd—O1—C6iv | 4.2 (6) | O4iv—Cd—O4—C3 | −49.9 (5) |
O4—Cd—O1—C6iv | −114.8 (6) | O1—Cd—O4—C3 | 10.4 (6) |
O1iv—Cd—O1—C6iv | −55.4 (6) | O1iv—Cd—O4—C3 | −110.2 (6) |
O1ii—Cd—O1—C6iv | 159.4 (6) | O1ii—Cd—O4—C3 | 93.3 (6) |
O1iii—Cd—O1—C6iv | 47.5 (6) | O1iii—Cd—O4—C3 | −152.9 (5) |
O4iii—Cd—O1—C2 | −29.6 (6) | O4iii—Cd—O4—C5 | −63.8 (5) |
O4ii—Cd—O1—C2 | −141.1 (5) | O4ii—Cd—O4—C5 | −175.0 (5) |
O4iv—Cd—O1—C2 | 134.9 (5) | O4iv—Cd—O4—C5 | 82.0 (5) |
O4—Cd—O1—C2 | 15.9 (5) | O1—Cd—O4—C5 | 142.2 (5) |
O1iv—Cd—O1—C2 | 75.3 (5) | O1iv—Cd—O4—C5 | 21.6 (5) |
O1ii—Cd—O1—C2 | −69.9 (5) | O1ii—Cd—O4—C5 | −134.8 (5) |
O1iii—Cd—O1—C2 | 178.2 (5) | O1iii—Cd—O4—C5 | −21.1 (6) |
C6iv—O1—C2—C3 | 91.3 (9) | C3—O4—C5—C6 | 86.1 (9) |
Cd—O1—C2—C3 | −41.2 (9) | Cd—O4—C5—C6 | −47.1 (9) |
O1—C2—C3—O4 | 50.4 (10) | O4—C5—C6—O1iv | 50.2 (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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