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In the title compound, [CdI
2(C
3H
8N
2O)
3], the Cd atom is five-coordinated by O atoms of three monodentate dimethylurea ligands and two iodide ligands. The coordination polyhedron is a distorted trigonal bipyramid of molecular symmetry
C2. Two dimethylurea ligands are involved in intermolecular N—H
O hydrogen bonds, whereas the third participates in N—H
I contacts.
Supporting information
CCDC reference: 647257
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (N-C) = 0.013 Å
- R factor = 0.047
- wR factor = 0.124
- Data-to-parameter ratio = 19.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O7
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.11
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
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); software used to prepare material for publication: WinGX (Farrugia, 1999).
Tris(1,3-dimethylurea)diiodidocadmium(II)
top
Crystal data top
[CdI2(C3H8N2O)3I2] | F(000) = 1192 |
Mr = 630.54 | Dx = 2.121 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 25 reflections |
a = 13.712 (9) Å | θ = 13–14° |
b = 8.807 (5) Å | µ = 4.25 mm−1 |
c = 17.265 (9) Å | T = 293 K |
β = 108.74 (5)° | Prism, colourless |
V = 1974 (2) Å3 | 0.10 × 0.10 × 0.10 mm |
Z = 4 | |
Data collection top
Enraf–Nonius CAD-4 diffractometer | Rint = 0.059 |
Radiation source: Enraf Nonius FR590 | θmax = 26.0°, θmin = 2.5° |
Graphite monochromator | h = −16→15 |
non–profiled ω scans | k = 0→10 |
1939 measured reflections | l = 0→21 |
1919 independent reflections | 1 standard reflections every 60 min |
1596 reflections with I > 2σ(I) | intensity decay: 1% |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.124 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0619P)2 + 19.5739P] where P = (Fo2 + 2Fc2)/3 |
1919 reflections | (Δ/σ)max < 0.001 |
100 parameters | Δρmax = 0.99 e Å−3 |
0 restraints | Δρmin = −0.74 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Cd1 | 0.0000 | 0.16105 (8) | 0.2500 | 0.0402 (2) | |
I1 | 0.06270 (4) | 0.30516 (6) | 0.39795 (4) | 0.0527 (2) | |
O1 | 0.1747 (4) | 0.1352 (6) | 0.2463 (3) | 0.0458 (12) | |
C2 | 0.2204 (6) | 0.0097 (8) | 0.2446 (6) | 0.0471 (19) | |
N3 | 0.2712 (6) | −0.0639 (9) | 0.3130 (5) | 0.063 (2) | |
H3 | 0.2949 | −0.1529 | 0.3093 | 0.076* | |
C4 | 0.2877 (10) | −0.0006 (13) | 0.3926 (7) | 0.082 (3) | |
H4A | 0.3253 | 0.0929 | 0.3976 | 0.122* | |
H4B | 0.3264 | −0.0709 | 0.4335 | 0.122* | |
H4C | 0.2225 | 0.0187 | 0.4003 | 0.122* | |
N5 | 0.2183 (6) | −0.0513 (9) | 0.1726 (5) | 0.064 (2) | |
H5 | 0.2436 | −0.1407 | 0.1728 | 0.077* | |
C6 | 0.1761 (10) | 0.0245 (14) | 0.0955 (6) | 0.082 (3) | |
H6A | 0.1100 | 0.0662 | 0.0917 | 0.123* | |
H6B | 0.1685 | −0.0468 | 0.0519 | 0.123* | |
H6C | 0.2216 | 0.1047 | 0.0914 | 0.123* | |
O7 | 0.0000 | −0.0854 (9) | 0.2500 | 0.076 (2) | |
C8 | 0.0000 | −0.2250 (15) | 0.2500 | 0.078 (2) | |
N9 | 0.0199 (9) | −0.3042 (10) | 0.3192 (7) | 0.090 (2) | |
H9 | 0.0191 | −0.4017 | 0.3166 | 0.108* | |
C10 | 0.0424 (13) | −0.2333 (16) | 0.3977 (8) | 0.105 (4) | |
H10A | 0.1154 | −0.2191 | 0.4210 | 0.157* | |
H10B | 0.0184 | −0.2968 | 0.4330 | 0.157* | |
H10C | 0.0085 | −0.1366 | 0.3916 | 0.157* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0396 (4) | 0.0319 (4) | 0.0562 (5) | 0.000 | 0.0253 (3) | 0.000 |
I1 | 0.0534 (4) | 0.0507 (3) | 0.0618 (4) | −0.0062 (2) | 0.0294 (3) | −0.0121 (2) |
O1 | 0.043 (3) | 0.034 (3) | 0.068 (3) | 0.006 (2) | 0.029 (3) | −0.005 (2) |
C2 | 0.039 (4) | 0.031 (4) | 0.080 (6) | −0.005 (3) | 0.031 (4) | −0.012 (4) |
N3 | 0.061 (5) | 0.046 (4) | 0.083 (5) | 0.024 (4) | 0.024 (4) | 0.007 (4) |
C4 | 0.097 (9) | 0.076 (7) | 0.078 (7) | 0.031 (6) | 0.036 (6) | 0.012 (6) |
N5 | 0.072 (5) | 0.048 (4) | 0.079 (5) | 0.022 (4) | 0.033 (4) | −0.015 (4) |
C6 | 0.093 (8) | 0.094 (9) | 0.069 (7) | 0.030 (7) | 0.039 (6) | 0.001 (6) |
O7 | 0.104 (6) | 0.018 (3) | 0.120 (6) | 0.000 | 0.054 (5) | 0.000 |
C8 | 0.109 (6) | 0.031 (4) | 0.108 (6) | 0.000 | 0.055 (5) | 0.000 |
N9 | 0.126 (6) | 0.047 (4) | 0.106 (5) | 0.001 (3) | 0.048 (5) | −0.002 (3) |
C10 | 0.139 (9) | 0.073 (6) | 0.103 (8) | 0.015 (7) | 0.040 (7) | −0.004 (6) |
Geometric parameters (Å, º) top
Cd1—O7 | 2.170 (8) | N5—H5 | 0.8600 |
Cd1—O1 | 2.428 (5) | C6—H6A | 0.9600 |
Cd1—I1 | 2.7319 (14) | C6—H6B | 0.9600 |
O1—C2 | 1.275 (9) | C6—H6C | 0.9600 |
C2—N3 | 1.331 (11) | O7—C8 | 1.230 (16) |
C2—N5 | 1.346 (11) | C8—N9 | 1.333 (12) |
N3—C4 | 1.432 (13) | N9—C10 | 1.432 (16) |
N3—H3 | 0.8600 | N9—H9 | 0.8600 |
C4—H4A | 0.9600 | C10—H10A | 0.9600 |
C4—H4B | 0.9600 | C10—H10B | 0.9600 |
C4—H4C | 0.9600 | C10—H10C | 0.9600 |
N5—C6 | 1.433 (13) | | |
| | | |
O7—Cd1—O1 | 84.61 (12) | C2—N5—H5 | 118.2 |
O1—Cd1—O1i | 169.2 (2) | C6—N5—H5 | 118.2 |
O1—Cd1—I1i | 92.05 (14) | N5—C6—H6A | 109.5 |
O7—Cd1—I1 | 117.68 (3) | N5—C6—H6B | 109.5 |
O1—Cd1—I1 | 92.95 (14) | H6A—C6—H6B | 109.5 |
I1i—Cd1—I1 | 124.64 (5) | N5—C6—H6C | 109.5 |
C2—O1—Cd1 | 125.4 (5) | H6A—C6—H6C | 109.5 |
O1—C2—N3 | 121.5 (8) | H6B—C6—H6C | 109.5 |
O1—C2—N5 | 120.1 (8) | C8—O7—Cd1 | 180 |
N3—C2—N5 | 118.4 (7) | O7—C8—N9 | 121.5 (6) |
C2—N3—C4 | 122.6 (8) | N9i—C8—N9 | 116.9 (13) |
C2—N3—H3 | 118.7 | C8—N9—C10 | 122.7 (10) |
C4—N3—H3 | 118.7 | C8—N9—H9 | 118.7 |
N3—C4—H4A | 109.5 | C10—N9—H9 | 118.7 |
N3—C4—H4B | 109.5 | N9—C10—H10A | 109.5 |
H4A—C4—H4B | 109.5 | N9—C10—H10B | 109.5 |
N3—C4—H4C | 109.5 | H10A—C10—H10B | 109.5 |
H4A—C4—H4C | 109.5 | N9—C10—H10C | 109.5 |
H4B—C4—H4C | 109.5 | H10A—C10—H10C | 109.5 |
C2—N5—C6 | 123.6 (8) | H10B—C10—H10C | 109.5 |
Symmetry code: (i) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N3—H3···O1ii | 0.86 | 2.20 | 3.019 (9) | 160 |
N5—H5···O1ii | 0.86 | 2.47 | 3.228 (9) | 148 |
N9—H9···I1iii | 0.86 | 2.91 | 3.677 (9) | 150 |
Symmetry codes: (ii) −x+1/2, y−1/2, −z+1/2; (iii) x, y−1, z. |
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