Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809052556/hb5231sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536809052556/hb5231Isup2.hkl |
CCDC reference: 749279
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.010 Å
- R factor = 0.029
- wR factor = 0.056
- Data-to-parameter ratio = 15.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT923_ALERT_1_B S values in the CIF and FCF Differ by ....... 0.03
Alert level C PLAT213_ALERT_2_C Atom C3 has ADP max/min Ratio ..... 3.40 prola PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Re1 -- I1 .. 7.70 su PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.66 PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang .. 10 PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 4 PLAT971_ALERT_2_C Large Calcd. Non-Metal Positive Residual Density 1.60 eA-3 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C11 H13 I2 N4 O2 Re PLAT922_ALERT_1_C wR2 * 100.0 in the CIF and FCF Differ by ....... 0.14 PLAT927_ALERT_1_C Reported and Calculated wR2 * 100.0 Differ by . -0.24
0 ALERT level A = In general: serious problem 1 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 4 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
A mixture of (NH4)2[ReI6] (prepared according to the literature procedure (Watt & Thompson, 1963) (0.12 g) and 0.30 g of 2,2,-(bipyrimidine) (from Aldrich) was added to a mixture of 2-propanol/acetone (1:1) (50 cm3) and then was stirred at 40° for about 4 h, the color of the solution was dark green. The solution was left for slow crystallization by evaporation under parafilm. The mixture was kept at room temperature for crystallization. After five days the pale green plate-shaped crystals were obtained. Anal. Calc. For: [ReOI2(C3H7O)(2,2,bipyrimidine)] C 19.62, H 2.08, N 8.32, I 37.69%: found C 19.01, H 1.89, N 8.15, I 37.50%. Selected IR data (KBr): 2925 (m), 2854 (m), 1717 (m), 1631 (m), 1610 (w), 1558 (s), 1464 (m), 1406 (s),1378 (m), 1271 (w), 1193 (w), 1191 (w), 978 (w), 908(w), 807 (w),645 (m), 561 (w), 535 (w), 452 (s), 390 (w), 358(w), 315 (s), 162 (versus), 131 (s), 74 (w).
TG–DTA Thermogravimetric measurements were carried out using a TG–DTA SETSYS 16Y18 device under nitrogen atmosphere for a sample placed in Al2O3 crucible. The investigated temperature range was from room temperature to 1400°C at 10°C/min. temperature changes rate. IR spectra The room temperature FT—IR spectra of polycrystalline samples were measured by means of the Bruker IFS-66 instrument.
The H atoms were generated geometrically and refined using a riding model, with C—H = 0.95 Å and Uiso(H) = 1.2 Ueq(C). The highest peak of 0.82 electrons at the difference Fourier map was situated near the Re atom.
Data collection: CrysAlis CCD (Oxford Diffraction, 2007); cell refinement: CrysAlis RED (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).
[Re(C3H7O)I2O(C8H6N4)] | F(000) = 1216 |
Mr = 673.26 | Dx = 2.847 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2115 reflections |
a = 10.3973 (3) Å | θ = 2.9–25.1° |
b = 10.9046 (3) Å | µ = 11.67 mm−1 |
c = 15.6341 (6) Å | T = 100 K |
β = 117.616 (2)° | Plate, pale green |
V = 1570.63 (9) Å3 | 0.12 × 0.11 × 0.03 mm |
Z = 4 |
Oxford Diffraction KM-4-CCD diffractometer | 2776 independent reflections |
Radiation source: fine-focus sealed tube | 2288 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
/w scans | θmax = 25.1°, θmin = 2.9° |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2007) | h = −12→12 |
Tmin = 0.456, Tmax = 0.611 | k = −11→12 |
15982 measured reflections | l = −18→18 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.056 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0251P)2 + 3.8665P] where P = (Fo2 + 2Fc2)/3 |
2776 reflections | (Δ/σ)max = 0.001 |
183 parameters | Δρmax = 1.85 e Å−3 |
0 restraints | Δρmin = −1.34 e Å−3 |
[Re(C3H7O)I2O(C8H6N4)] | V = 1570.63 (9) Å3 |
Mr = 673.26 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 10.3973 (3) Å | µ = 11.67 mm−1 |
b = 10.9046 (3) Å | T = 100 K |
c = 15.6341 (6) Å | 0.12 × 0.11 × 0.03 mm |
β = 117.616 (2)° |
Oxford Diffraction KM-4-CCD diffractometer | 2776 independent reflections |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2007) | 2288 reflections with I > 2σ(I) |
Tmin = 0.456, Tmax = 0.611 | Rint = 0.050 |
15982 measured reflections |
R[F2 > 2σ(F2)] = 0.029 | 0 restraints |
wR(F2) = 0.056 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.85 e Å−3 |
2776 reflections | Δρmin = −1.34 e Å−3 |
183 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Re1 | 0.26746 (3) | −0.33250 (2) | −0.10973 (2) | 0.02512 (9) | |
I1 | 0.13432 (6) | −0.31460 (4) | −0.30538 (3) | 0.03659 (14) | |
I2 | 0.22482 (5) | −0.57955 (4) | −0.12777 (3) | 0.03021 (13) | |
O1 | 0.4380 (5) | −0.3317 (4) | −0.0984 (3) | 0.0228 (10) | |
O2 | 0.0941 (5) | −0.3139 (4) | −0.1035 (3) | 0.0317 (11) | |
N1 | 0.2890 (6) | −0.1369 (5) | −0.0790 (4) | 0.0228 (12) | |
N2 | 0.3689 (7) | −0.3247 (5) | 0.0476 (4) | 0.0281 (13) | |
N3 | 0.3837 (7) | 0.0063 (5) | 0.0504 (4) | 0.0293 (14) | |
N4 | 0.4828 (7) | −0.1874 (5) | 0.1792 (4) | 0.0316 (15) | |
C1 | 0.2343 (8) | −0.0453 (6) | −0.1436 (5) | 0.0324 (17) | |
H1 | 0.1832 | −0.0636 | −0.2105 | 0.039* | |
C2 | 0.2519 (9) | 0.0735 (6) | −0.1134 (5) | 0.0365 (19) | |
H2 | 0.2114 | 0.1388 | −0.1583 | 0.044* | |
C3 | 0.3303 (8) | 0.0959 (6) | −0.0157 (5) | 0.0328 (18) | |
H3 | 0.3473 | 0.1786 | 0.0057 | 0.039* | |
C4 | 0.5150 (9) | −0.2833 (6) | 0.2389 (5) | 0.0342 (18) | |
H4 | 0.5655 | −0.2690 | 0.3065 | 0.041* | |
C5 | 0.4775 (8) | −0.4035 (6) | 0.2062 (5) | 0.0320 (17) | |
H5 | 0.5002 | −0.4704 | 0.2498 | 0.038* | |
C6 | 0.4065 (8) | −0.4201 (6) | 0.1084 (5) | 0.0273 (16) | |
H6 | 0.3834 | −0.5009 | 0.0830 | 0.033* | |
C7 | 0.3584 (8) | −0.1071 (6) | 0.0158 (5) | 0.0291 (17) | |
C8 | 0.4078 (8) | −0.2118 (6) | 0.0862 (5) | 0.0261 (16) | |
C9 | −0.0043 (9) | −0.2989 (8) | −0.0654 (6) | 0.045 (2) | |
H9 | 0.0494 | −0.3159 | 0.0055 | 0.054* | |
C10 | −0.1237 (9) | −0.3889 (8) | −0.1089 (6) | 0.043 (2) | |
H10A | −0.1895 | −0.3648 | −0.1754 | 0.065* | |
H10B | −0.1773 | −0.3915 | −0.0713 | 0.065* | |
H10C | −0.0834 | −0.4703 | −0.1087 | 0.065* | |
C11 | −0.0531 (8) | −0.1652 (6) | −0.0783 (6) | 0.0382 (18) | |
H11A | 0.0309 | −0.1123 | −0.0416 | 0.057* | |
H11B | −0.1249 | −0.1540 | −0.0549 | 0.057* | |
H11C | −0.0966 | −0.1434 | −0.1469 | 0.057* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.03734 (18) | 0.00899 (14) | 0.03104 (16) | 0.00073 (12) | 0.01756 (13) | 0.00019 (11) |
I1 | 0.0430 (3) | 0.0213 (3) | 0.0286 (2) | 0.0025 (2) | 0.0023 (2) | 0.0026 (2) |
I2 | 0.0453 (3) | 0.0095 (2) | 0.0337 (3) | −0.00078 (19) | 0.0165 (2) | −0.00140 (18) |
O1 | 0.031 (3) | 0.015 (2) | 0.022 (2) | 0.0001 (19) | 0.011 (2) | −0.0019 (19) |
O2 | 0.041 (3) | 0.016 (2) | 0.041 (3) | 0.002 (2) | 0.022 (3) | −0.001 (2) |
N1 | 0.030 (3) | 0.013 (3) | 0.028 (3) | 0.001 (2) | 0.016 (3) | 0.000 (2) |
N2 | 0.045 (4) | 0.012 (3) | 0.034 (3) | 0.001 (3) | 0.025 (3) | 0.001 (3) |
N3 | 0.056 (4) | 0.012 (3) | 0.036 (3) | −0.005 (3) | 0.035 (3) | −0.004 (3) |
N4 | 0.065 (4) | 0.018 (3) | 0.027 (3) | −0.003 (3) | 0.034 (3) | −0.001 (2) |
C1 | 0.049 (5) | 0.016 (4) | 0.029 (4) | 0.008 (3) | 0.015 (4) | 0.002 (3) |
C2 | 0.062 (5) | 0.011 (4) | 0.045 (5) | 0.005 (4) | 0.033 (4) | 0.009 (3) |
C3 | 0.061 (5) | 0.006 (3) | 0.050 (5) | −0.002 (3) | 0.042 (4) | −0.002 (3) |
C4 | 0.065 (6) | 0.021 (4) | 0.025 (4) | −0.001 (4) | 0.028 (4) | 0.000 (3) |
C5 | 0.055 (5) | 0.024 (4) | 0.030 (4) | 0.004 (3) | 0.030 (4) | 0.001 (3) |
C6 | 0.043 (5) | 0.010 (3) | 0.038 (4) | −0.002 (3) | 0.026 (4) | −0.003 (3) |
C7 | 0.048 (5) | 0.011 (4) | 0.044 (4) | −0.002 (3) | 0.034 (4) | −0.004 (3) |
C8 | 0.045 (5) | 0.010 (3) | 0.037 (4) | −0.001 (3) | 0.030 (4) | −0.001 (3) |
C9 | 0.042 (5) | 0.045 (5) | 0.039 (4) | 0.004 (4) | 0.013 (4) | −0.004 (4) |
C10 | 0.041 (5) | 0.050 (5) | 0.039 (4) | −0.010 (4) | 0.019 (4) | −0.009 (4) |
C11 | 0.034 (4) | 0.026 (4) | 0.051 (5) | 0.007 (3) | 0.016 (4) | 0.001 (4) |
Re1—O1 | 1.698 (4) | C2—H2 | 0.9500 |
Re1—O2 | 1.861 (5) | C3—H3 | 0.9500 |
Re1—N1 | 2.175 (5) | C4—C5 | 1.395 (10) |
Re1—N2 | 2.183 (6) | C4—H4 | 0.9500 |
Re1—I1 | 2.7176 (5) | C5—C6 | 1.368 (10) |
Re1—I2 | 2.7235 (5) | C5—H5 | 0.9500 |
O2—C9 | 1.411 (10) | C6—H6 | 0.9500 |
N1—C1 | 1.345 (8) | C7—C8 | 1.502 (10) |
N1—C7 | 1.353 (9) | C9—C10 | 1.478 (11) |
N2—C6 | 1.339 (8) | C9—C11 | 1.526 (10) |
N2—C8 | 1.348 (8) | C9—H9 | 1.0000 |
N3—C7 | 1.326 (8) | C10—H10A | 0.9800 |
N3—C3 | 1.341 (9) | C10—H10B | 0.9800 |
N4—C8 | 1.320 (9) | C10—H10C | 0.9800 |
N4—C4 | 1.337 (9) | C11—H11A | 0.9800 |
C1—C2 | 1.361 (10) | C11—H11B | 0.9800 |
C1—H1 | 0.9500 | C11—H11C | 0.9800 |
C2—C3 | 1.380 (10) | ||
O1—Re1—O2 | 169.68 (19) | N4—C4—C5 | 122.8 (6) |
O1—Re1—N1 | 88.66 (19) | N4—C4—H4 | 118.6 |
O2—Re1—N1 | 83.34 (19) | C5—C4—H4 | 118.6 |
O1—Re1—N2 | 86.9 (2) | C6—C5—C4 | 116.6 (6) |
O2—Re1—N2 | 84.9 (2) | C6—C5—H5 | 121.7 |
N1—Re1—N2 | 76.5 (2) | C4—C5—H5 | 121.7 |
O1—Re1—I1 | 94.56 (13) | N2—C6—C5 | 121.3 (6) |
O2—Re1—I1 | 92.91 (15) | N2—C6—H6 | 119.4 |
N1—Re1—I1 | 97.18 (14) | C5—C6—H6 | 119.4 |
N2—Re1—I1 | 173.47 (14) | N3—C7—N1 | 125.1 (6) |
O1—Re1—I2 | 97.35 (14) | N3—C7—C8 | 118.3 (6) |
O2—Re1—I2 | 89.91 (13) | N1—C7—C8 | 116.6 (6) |
N1—Re1—I2 | 171.11 (14) | N4—C8—N2 | 125.3 (6) |
N2—Re1—I2 | 97.22 (14) | N4—C8—C7 | 118.7 (6) |
I1—Re1—I2 | 88.908 (16) | N2—C8—C7 | 115.9 (6) |
C9—O2—Re1 | 160.7 (5) | O2—C9—C10 | 110.3 (6) |
C1—N1—C7 | 118.0 (5) | O2—C9—C11 | 108.4 (7) |
C1—N1—Re1 | 126.7 (4) | C10—C9—C11 | 114.6 (7) |
C7—N1—Re1 | 115.2 (4) | O2—C9—H9 | 107.7 |
C6—N2—C8 | 117.7 (6) | C10—C9—H9 | 107.7 |
C6—N2—Re1 | 126.8 (4) | C11—C9—H9 | 107.7 |
C8—N2—Re1 | 115.3 (4) | C9—C10—H10A | 109.5 |
C7—N3—C3 | 115.6 (6) | C9—C10—H10B | 109.5 |
C8—N4—C4 | 116.2 (6) | H10A—C10—H10B | 109.5 |
N1—C1—C2 | 120.3 (7) | C9—C10—H10C | 109.5 |
N1—C1—H1 | 119.8 | H10A—C10—H10C | 109.5 |
C2—C1—H1 | 119.8 | H10B—C10—H10C | 109.5 |
C1—C2—C3 | 117.9 (7) | C9—C11—H11A | 109.5 |
C1—C2—H2 | 121.1 | C9—C11—H11B | 109.5 |
C3—C2—H2 | 121.1 | H11A—C11—H11B | 109.5 |
N3—C3—C2 | 123.1 (6) | C9—C11—H11C | 109.5 |
N3—C3—H3 | 118.5 | H11A—C11—H11C | 109.5 |
C2—C3—H3 | 118.5 | H11B—C11—H11C | 109.5 |
O1—Re1—O2—C9 | −37 (2) | C1—C2—C3—N3 | −3.1 (11) |
N1—Re1—O2—C9 | −76.5 (14) | C8—N4—C4—C5 | 2.4 (11) |
N2—Re1—O2—C9 | 0.5 (14) | N4—C4—C5—C6 | 0.8 (11) |
I1—Re1—O2—C9 | −173.4 (14) | C8—N2—C6—C5 | 2.2 (10) |
I2—Re1—O2—C9 | 97.7 (14) | Re1—N2—C6—C5 | 176.0 (5) |
O1—Re1—N1—C1 | 100.5 (6) | C4—C5—C6—N2 | −3.2 (10) |
O2—Re1—N1—C1 | −86.0 (6) | C3—N3—C7—N1 | 2.4 (10) |
N2—Re1—N1—C1 | −172.3 (6) | C3—N3—C7—C8 | −176.6 (6) |
I1—Re1—N1—C1 | 6.1 (6) | C1—N1—C7—N3 | −3.6 (10) |
O1—Re1—N1—C7 | −83.2 (5) | Re1—N1—C7—N3 | 179.7 (5) |
O2—Re1—N1—C7 | 90.2 (5) | C1—N1—C7—C8 | 175.4 (6) |
N2—Re1—N1—C7 | 3.9 (4) | Re1—N1—C7—C8 | −1.3 (7) |
I1—Re1—N1—C7 | −177.7 (4) | C4—N4—C8—N2 | −3.7 (11) |
O1—Re1—N2—C6 | −91.0 (6) | C4—N4—C8—C7 | 175.4 (6) |
O2—Re1—N2—C6 | 95.2 (6) | C6—N2—C8—N4 | 1.5 (11) |
N1—Re1—N2—C6 | 179.6 (6) | Re1—N2—C8—N4 | −173.1 (6) |
I2—Re1—N2—C6 | 6.0 (6) | C6—N2—C8—C7 | −177.6 (6) |
O1—Re1—N2—C8 | 83.0 (5) | Re1—N2—C8—C7 | 7.8 (8) |
O2—Re1—N2—C8 | −90.8 (5) | N3—C7—C8—N4 | −4.5 (10) |
N1—Re1—N2—C8 | −6.4 (5) | N1—C7—C8—N4 | 176.4 (6) |
I2—Re1—N2—C8 | 180.0 (5) | N3—C7—C8—N2 | 174.7 (6) |
C7—N1—C1—C2 | 1.3 (11) | N1—C7—C8—N2 | −4.4 (9) |
Re1—N1—C1—C2 | 177.5 (5) | Re1—O2—C9—C10 | −130.8 (12) |
N1—C1—C2—C3 | 1.8 (11) | Re1—O2—C9—C11 | 102.9 (14) |
C7—N3—C3—C2 | 1.1 (10) |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···I1 | 0.95 | 3.04 | 3.697 (7) | 127 |
C6—H6···I2 | 0.95 | 3.05 | 3.709 (7) | 128 |
C5—H5···N4i | 0.95 | 2.58 | 3.504 (9) | 163 |
C6—H6···O1ii | 0.95 | 2.53 | 3.193 (9) | 127 |
C9—H9···I1iii | 1.00 | 3.02 | 3.834 (8) | 139 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1, −y−1, −z; (iii) x, −y−1/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Re(C3H7O)I2O(C8H6N4)] |
Mr | 673.26 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 100 |
a, b, c (Å) | 10.3973 (3), 10.9046 (3), 15.6341 (6) |
β (°) | 117.616 (2) |
V (Å3) | 1570.63 (9) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 11.67 |
Crystal size (mm) | 0.12 × 0.11 × 0.03 |
Data collection | |
Diffractometer | Oxford Diffraction KM-4-CCD diffractometer |
Absorption correction | Analytical (CrysAlis RED; Oxford Diffraction, 2007) |
Tmin, Tmax | 0.456, 0.611 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15982, 2776, 2288 |
Rint | 0.050 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.029, 0.056, 1.03 |
No. of reflections | 2776 |
No. of parameters | 183 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.85, −1.34 |
Computer programs: CrysAlis CCD (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005).
Re1—O1 | 1.698 (4) | Re1—N2 | 2.183 (6) |
Re1—O2 | 1.861 (5) | Re1—I1 | 2.7176 (5) |
Re1—N1 | 2.175 (5) | Re1—I2 | 2.7235 (5) |
N1—Re1—N2 | 76.5 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
C1—H1···I1 | 0.95 | 3.04 | 3.697 (7) | 127 |
C6—H6···I2 | 0.95 | 3.05 | 3.709 (7) | 128 |
C5—H5···N4i | 0.95 | 2.58 | 3.504 (9) | 163 |
C6—H6···O1ii | 0.95 | 2.53 | 3.193 (9) | 127 |
C9—H9···I1iii | 1.00 | 3.02 | 3.834 (8) | 139 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1, −y−1, −z; (iii) x, −y−1/2, z+1/2. |
ReV complexes have been research object for many authors during the last years. Complexes of general formula [ReOX2(C5H4N)CH(O)CH2(C5H4N)] (X = Cl, I) were obtained by a reaction of trans-[ReOCl3(PPh3)2] and trans-[ReOI2(OEt)(PPh3)2] with cis-1,2-di-(2-pyridyl)ethylene (DPE) in ethanol and in benzene on air. The coordinated DPE ligand undergoes addition of water at the ethylene carbon atoms, and the (C5H4N)CH(O)CH2(C5H4N) moiety acts as terdentate N,O,N-donor ligand. X-ray crystal structures of both complexes have been determined and show distorted octahedral geometry around the rhenium(V) centre (Abrahams et al., 2005). Complexes cis-[ReOX2(msa)(PPh3)] [X = Cl(1), I(2)] were prepared from trans-[ReOCl3(PPh3)2] or trans-[ReOI2(OEt)(PPh3)2] in reaction with 2-(1-iminoethyl)phenol (Hmsa) in acetonitrile. X-ray crystal structure shows, that the bonding distances and angles in 1 and 2 are nearly identical, and that the two halide ligands in each complex are coordinated cis to each other in the equatorial plane cis to the oxido group. Rhenium(V) complexes with two iodido ligands cis to each other are rare (Abrahams et al., 2007). Rhenium(V) complexes with trans-O—Re-(2-propoxido) core are known. Rhenium(V) complex with 2-propoxido ligand of formula [ReOCl2(C3H7O)(Ph3P)2] has been synthesized (Abram et al. 1995), and the other one, [ReClO(C3H7O)PPh3L] (where L = pyridine-2-thiolato ligand), was obtained (Schmidt-Brucken & Abram, 2000). This paper contains a report on the synthesis and structure of the first characterized [ReOI2(C3H7O)(2–2?bipyrimidine)] 1 complex with ReI2 core and 2-propoxido ligand. Fig. 1 presents the view of molecular structure of compound 1, the compound crystallizes in monoclinic crystal system in P21/c space group. The compound was obtained in the synthesis with (NH4)2ReI6 and 2,2'-bipyrimidine as substrates in a mixture of 2-propanol and acetone. The environment around the metal center is a distorted octahedron, with two iodido ligands, 2-propoxido ligand and 2,2'-bipyrimidine ligand coordinated via nitrogen atoms. The Re—I bond lengths are Re1—I1 2.7176 (5) Å, Re1—I2 2.7235 (5) Å, respectively,similar Re—I distances were observed in 2-(2-aminophenyl)ethanolato-N,O)-bis(iododo)-oxido- triphenylphosphine-rhenium(V) and diodido-(3-hydroxidopicolinato)-oxido-)-triphenylphosphine-rhenium(II) (Gerber et al., 2004, Quintal et al., 2000). On the other hand, the Re1—O1 1.698 (4) Å bond length is characteristic for monooxido-rhenium(V) complexes (on average 1.69%A), which is in agreement with the situation in the comparable complexes (Graziani et al., 1985, Lebuis et al., 1993). The O atom from 2-propoxido ligand is coordinated to the rhenium atom with Re—O2 1.861 (5) Å; this bond is remarkably short with the same multiple bond character as discussed (Ciani et al. 1983). The O—Re—O unit is nearly linear with an angle of 169.69 (3)°. Moreover, a molecule of 2,2'-bipyrimidine is coordinated with Re—N bond length of Re1—N1 2.175 (5) %A, Re1—N2 2.183 (6) Å, which is comparable to the previously investigated trans-[ReCl4(py)2] (Mrozinski et al., 2002, Herrman et al., 1990). Re atom lies within the plane of I1, I2, N1, N2 atoms, the N1—Re1—O1 and N2—Re1—O1 angles are 88.63 (19), 86.93 (14) and N1—Re1—O2, N2—Re1—O2 83.37 (14) and 84.87 (15) and are directed in side to 2,2'-bipyrimidine. The rings of the 4,4'-bpy ligand are coplanar with the plane defined by the I ligands, one of the Re—N bond is shorter (Re1—N1 2.175 (5) Å, Re1—N2 2.183 (6) Å), which may be a result of iodido ligand presence. The molecule conformation is stabilized by intramolecular hydrogen bonds C(1)—H(1)···I(1) and C(6)—-H(6)···I(2), as well as by the intermolecular hydrogen bonds of C—H···O and C—H···N type. All hydrogen bonds are summarized in Table 2. In the crystal structure packing along [100] and [010] a layered arrangement of the molecules could be observed. The crystal structure packing viewed along [100] direction is illustrated in Fig. 2. In the structure the stacking interactions are observed. pi-pi stacking interactions between the 2,2'-bypirymidine rings contribute to forming a supramolecular network structure (Fig. 2). The centroid-centroid distance of the adjacent aromatic rings is about 3.58%A, indicating a normal pi-pi interaction. The corresponding TG-DTA curves (the measurement was carried out under nitrogen atmosphere) for the title compound (Fig. 3) show a three-step decomposition process and that the compound is very stable during heating. In the first step of the thermal decomposition process weight loss in the temperature range 242–247°C of 1.39% (calc. 1.43%) is observed. In DTA curve, this decomposition is visible as an endothermic peak at temperature 247°C, indicating the presence of coordinated 4.4,-bipyrimidine (corresponding to the weight loss of 1.39% in thermal decomposition, which is in agreement with the calculated value of 1.43%). Further weight losses correspond to decomposition of further compound parts, they are continuous and are difficult for unambiguous interpretation (decomposition of all compound constituents except for rhenium part). Another peak at 800°C is also observed, however, it is difficult to interpret. It is possible, that the decomposition process leads to rhenium oxides. Similar decomposition process through many intermediate stages has been observed for (NH4)2[Re3Cl12] (Irmler et al., 1991). In conclusion, an interesting rhenium(V) trans-2,2,-bipyrimidine-diiodido-oxido-(2-propoxido)-rhenium(V) complex with 2-propoxido ligand was obtained. The crystal structure is stabilized by hydrogen bonding interactions. This is the first structural report confirming the existence of a iodido rhenium complex with an aromatic amine and 2-propoxido ligand in coordination sphere.