A woven structure of hexa­acetamidecadmium(II) polyiodide

The coordination of the [Cd(acetamide)₆]²⁺ cation in the title compound, hexa­acetamideca­dmium(II) bis­(triiodide) bis(diiodine), [Cd(C₂H₅NO)₆](I₃)₂·2I₂, is octa­hedral. The I atoms form a woven structure consisting of alternating triidodide anions and iodine mol­ecules. Cd atoms and triiodide anions lie on inversion centres.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.023 Å
• R factor = 0.048
• wR factor = 0.083
• Data-to-parameter ratio = 22.0

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT431_ALERT_2_A Short Inter HL..A Contact  I2     ..  I3      ..       3.44 Ang.

Author Response: See Comment!

Alert level B
PLAT342_ALERT_3_B Low Bond Precision on C-C bonds (x 1000) Ang ...         23
PLAT431_ALERT_2_B Short Inter HL..A Contact  I1     ..  I5      ..       3.47 Ang.

Author Response: See Comment!

Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.97
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.98
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        Cd1
PLAT420_ALERT_2_C D-H Without Acceptor       N1A    -   H12A   ...          ?
PLAT420_ALERT_2_C D-H Without Acceptor       N1C    -   H12C   ...          ?
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.22 Ratio

   1 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   9 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Bruno et al., 2002); software used to prepare material for publication: WinGX (Farrugia, 1999).

Hexaacetamidecadmium Triiodide Adduct with Two Iodine Molecules

Crystal data

[Cd(C2H5NO)6](I3)2·2I2	Z = 1
Mr = 1735.82	F(000) = 770
Triclinic, P1	Dx = 2.911 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.666 (4) Å	Cell parameters from 25 reflections
b = 11.9817 (19) Å	θ = 12–13°
c = 12.426 (3) Å	µ = 8.38 mm^−1
α = 65.747 (15)°	T = 293 K
β = 80.79 (5)°	Prism, dark green
γ = 72.25 (3)°	0.11 × 0.10 × 0.09 mm
V = 990.3 (6) Å^3

Data collection

Enraf–Nonius CAD-4 diffractometer	2051 reflections with I > 2σ(I)
Radiation source: Enraf Nonius FR590	Rint = 0.000
Graphite monochromator	θmax = 25.7°, θmin = 1.8°
non–profiled ω scans	h = −8→9
Absorption correction: ψ scan (North et al., 1968)	k = −12→14
Tmin = 0.386, Tmax = 0.481	l = 0→15
3644 measured reflections	1 standard reflections every 60 min
3644 independent reflections	intensity decay: 2%

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.048	H-atom parameters constrained
wR(F^2) = 0.083	w = 1/[σ^2(Fo^2) + (0.017P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.87	(Δ/σ)max < 0.001
3644 reflections	Δρmax = 1.77 e Å^−3
166 parameters	Δρmin = −1.60 e Å^−3
Primary atom site location: structure-invariant direct methods

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Cd1	0.5000	0.5000	0.0000	0.0110 (3)
I1	0.7302 (2)	0.37092 (10)	0.46221 (11)	0.0449 (4)
I2	0.80870 (17)	0.60152 (10)	0.35408 (9)	0.0306 (3)
I3	0.8748 (2)	0.90028 (12)	0.24607 (11)	0.0482 (4)
I4	1.0000	1.0000	0.0000	0.0274 (4)
I5	0.64454 (17)	0.07588 (10)	0.61395 (10)	0.0371 (3)
I6	1.0000	0.0000	0.5000	0.0252 (4)
O1A	0.3524 (14)	0.4220 (9)	0.1787 (8)	0.022 (2)
C1A	0.390 (2)	0.3175 (13)	0.2613 (12)	0.026 (3)
N1A	0.5426 (18)	0.2224 (12)	0.2721 (11)	0.032 (3)
H11A	0.6279	0.2310	0.2175	0.038*
H12A	0.5554	0.1528	0.3337	0.038*
C2A	0.268 (2)	0.2932 (14)	0.3702 (12)	0.028 (4)
H21A	0.1427	0.3235	0.3487	0.042*
H22A	0.2879	0.3367	0.4152	0.042*
H23A	0.2964	0.2036	0.4169	0.042*
O1B	0.2461 (14)	0.6541 (10)	−0.0639 (9)	0.030 (3)
C1B	0.0775 (19)	0.6731 (14)	−0.0483 (13)	0.027 (3)
N1B	−0.0027 (18)	0.6037 (12)	0.0517 (10)	0.029 (3)
H11B	0.0638	0.5436	0.1076	0.035*
H12B	−0.1202	0.6197	0.0594	0.035*
C2B	−0.0588 (19)	0.7610 (13)	−0.1399 (12)	0.021 (3)
H21B	−0.0989	0.8425	−0.1342	0.031*
H22B	−0.1622	0.7271	−0.1276	0.031*
H23B	−0.0032	0.7698	−0.2169	0.031*
O1C	0.4115 (15)	0.3587 (10)	−0.0540 (9)	0.032 (3)
C1C	0.513 (2)	0.2894 (15)	−0.1042 (14)	0.036 (3)
N1C	0.6405 (18)	0.3297 (14)	−0.1900 (11)	0.037 (3)
H11C	0.6527	0.4049	−0.2112	0.045*
H12C	0.7086	0.2799	−0.2231	0.045*
C2C	0.464 (3)	0.1682 (17)	−0.0699 (16)	0.048 (5)
H21C	0.4258	0.1388	0.0121	0.072*
H22C	0.5688	0.1058	−0.0829	0.072*
H23C	0.3658	0.1817	−0.1168	0.072*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cd1	0.0170 (7)	0.0034 (5)	0.0087 (7)	−0.0001 (5)	−0.0049 (5)	0.0011 (5)
I1	0.0647 (9)	0.0058 (5)	0.0476 (8)	0.0037 (5)	−0.0150 (7)	0.0012 (5)
I2	0.0433 (7)	0.0202 (5)	0.0212 (6)	−0.0021 (5)	−0.0099 (5)	−0.0025 (4)
I3	0.0824 (10)	0.0255 (6)	0.0346 (7)	−0.0217 (6)	−0.0091 (7)	−0.0017 (5)
I4	0.0335 (8)	0.0163 (6)	0.0287 (8)	−0.0036 (6)	−0.0115 (6)	−0.0034 (6)
I5	0.0441 (7)	0.0180 (5)	0.0359 (7)	−0.0038 (5)	−0.0044 (5)	0.0005 (5)
I6	0.0429 (9)	0.0086 (6)	0.0160 (8)	−0.0036 (6)	−0.0076 (7)	0.0031 (6)
O1A	0.026 (5)	0.009 (4)	0.023 (5)	−0.002 (4)	−0.004 (4)	0.001 (4)
C1A	0.031 (5)	0.018 (5)	0.026 (5)	−0.002 (4)	−0.004 (4)	−0.008 (4)
N1A	0.036 (6)	0.024 (5)	0.029 (6)	−0.002 (5)	−0.002 (5)	−0.008 (4)
C2A	0.031 (6)	0.022 (6)	0.027 (6)	0.000 (5)	−0.004 (5)	−0.007 (5)
O1B	0.027 (5)	0.027 (5)	0.027 (5)	−0.005 (4)	−0.005 (4)	−0.003 (4)
C1B	0.031 (5)	0.027 (5)	0.026 (5)	−0.008 (4)	−0.005 (4)	−0.011 (4)
N1B	0.035 (6)	0.028 (5)	0.019 (5)	0.000 (5)	−0.005 (5)	−0.008 (4)
C2B	0.023 (6)	0.022 (5)	0.023 (6)	−0.010 (5)	−0.003 (5)	−0.011 (5)
O1C	0.038 (5)	0.027 (5)	0.033 (5)	−0.011 (4)	−0.002 (4)	−0.013 (4)
C1C	0.033 (5)	0.037 (5)	0.035 (5)	−0.010 (5)	−0.002 (5)	−0.010 (4)
N1C	0.033 (6)	0.036 (6)	0.037 (6)	−0.014 (5)	0.005 (5)	−0.008 (5)
C2C	0.047 (7)	0.047 (7)	0.048 (7)	−0.017 (6)	−0.010 (6)	−0.011 (6)

Geometric parameters (Å, º)

Cd1—O1B	2.220 (11)	C2A—H22A	0.9600
Cd1—O1B^i	2.220 (11)	C2A—H23A	0.9600
Cd1—O1A	2.285 (9)	O1B—C1B	1.239 (16)
Cd1—O1A^i	2.285 (9)	C1B—N1B	1.354 (16)
Cd1—O1C	2.357 (11)	C1B—C2B	1.491 (17)
Cd1—O1C^i	2.357 (11)	N1B—H11B	0.8600
I1—I2	2.7398 (17)	N1B—H12B	0.8600
I3—I4	2.9081 (17)	C2B—H21B	0.9600
I5—I6	2.927 (2)	C2B—H22B	0.9600
I1—I5	3.4680 (18)	C2B—H23B	0.9600
I2—I3	3.4371 (18)	O1C—C1C	1.250 (16)
I6—I5^ii	2.927 (2)	C1C—N1C	1.362 (17)
I4—I3^iii	2.9081 (17)	C1C—C2C	1.485 (19)
O1A—C1A	1.235 (15)	N1C—H11C	0.8600
C1A—N1A	1.342 (16)	N1C—H12C	0.8600
C1A—C2A	1.490 (16)	C2C—H21C	0.9600
N1A—H11A	0.8600	C2C—H22C	0.9600
N1A—H12A	0.8600	C2C—H23C	0.9600
C2A—H21A	0.9600
O1B—Cd1—O1B^i	180.0 (6)	H21A—C2A—H22A	109.5
O1B—Cd1—O1A	89.2 (3)	C1A—C2A—H23A	109.5
O1B^i—Cd1—O1A	90.8 (3)	H21A—C2A—H23A	109.5
O1B—Cd1—O1A^i	90.8 (3)	H22A—C2A—H23A	109.5
O1B^i—Cd1—O1A^i	89.2 (3)	C1B—O1B—Cd1	139.6 (10)
O1A—Cd1—O1A^i	180.0 (5)	O1B—C1B—N1B	122.7 (14)
O1B—Cd1—O1C	93.4 (4)	O1B—C1B—C2B	125.1 (13)
O1B^i—Cd1—O1C	86.6 (4)	N1B—C1B—C2B	111.8 (12)
O1A—Cd1—O1C	87.5 (4)	C1B—N1B—H11B	120.0
O1A^i—Cd1—O1C	92.5 (4)	C1B—N1B—H12B	120.0
O1B—Cd1—O1C^i	86.6 (4)	H11B—N1B—H12B	120.0
O1B^i—Cd1—O1C^i	93.4 (4)	C1B—C2B—H21B	109.5
O1A—Cd1—O1C^i	92.5 (4)	C1B—C2B—H22B	109.5
O1A^i—Cd1—O1C^i	87.5 (4)	H21B—C2B—H22B	109.5
O1C—Cd1—O1C^i	180.0 (4)	C1B—C2B—H23B	109.5
I1—I5—I6	80.49 (5)	H21B—C2B—H23B	109.5
I2—I3—I4	116.69 (5)	H22B—C2B—H23B	109.5
I2—I1—I5	176.51 (6)	C1C—O1C—Cd1	125.5 (11)
I1—I2—I3	172.93 (5)	O1C—C1C—N1C	122.0 (15)
I3—I4—I3^iii	180.00 (5)	O1C—C1C—C2C	112.6 (14)
I5—I6—I5^ii	180.000 (1)	N1C—C1C—C2C	125.0 (15)
C1A—O1A—Cd1	131.1 (10)	C1C—N1C—H11C	120.0
O1A—C1A—N1A	127.3 (14)	C1C—N1C—H12C	120.0
O1A—C1A—C2A	119.6 (13)	H11C—N1C—H12C	120.0
N1A—C1A—C2A	112.8 (12)	C1C—C2C—H21C	109.5
C1A—N1A—H11A	120.0	C1C—C2C—H22C	109.5
C1A—N1A—H12A	120.0	H21C—C2C—H22C	109.5
H11A—N1A—H12A	120.0	C1C—C2C—H23C	109.5
C1A—C2A—H21A	109.5	H21C—C2C—H23C	109.5
C1A—C2A—H22A	109.5	H22C—C2C—H23C	109.5

Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+2, −y, −z+1; (iii) −x+2, −y+2, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1A—H11A···O1B^i	0.86	2.13	2.912 (17)	151
N1B—H11B···O1A	0.86	2.32	3.095 (18)	149
N1B—H12B···O1C^iv	0.86	2.18	3.024 (19)	168
N1C—H11C···O1A^i	0.86	2.26	3.05 (2)	154

Symmetry codes: (i) −x+1, −y+1, −z; (iv) −x, −y+1, −z.