metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
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ISSN: 2056-9890
Volume 64| Part 10| October 2008| Pages m1226-m1227

Aqua­tricarbon­yl(4-carb­oxy­pyridine-2-carboxyl­ato-κ2N,O2)rhenium(I)

aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
*Correspondence e-mail: visserhg.sci@ufs.ac.za

(Received 25 July 2008; accepted 28 August 2008; online 6 September 2008)

There are two mol­ecules with similar bond dimensions in the asymmetric unit of the title complex, [Re(C7H4NO4)(CO)3(H2O)]. The metal centre is coordinated facially by three carbonyl groups, is chelated by a 4-carboxy­pyridine-2-carboxyl­ate ligand and is also coordinated by a water mol­ecule. O—H⋯O hydrogen bonds give rise to a three-dimensional network.

Related literature

For the monoclinic polymorph of the title compound, see: Mundwiler et al. (2004[Mundwiler, S., Kundig, M., Ortner, K. & Alberto, R. (2004). Dalton Trans. pp. 1320-1328.]). For related structures, see: Kemp (2006[Kemp, G. (2006). PhD thesis, University of Johannesburg, South Africa.]); Roodt et al. (2003[Roodt, A., Otto, S. & Steyl, G. (2003). Coord. Chem. Rev. 245, 121-129.]); Schutte et al. (2007[Schutte, M., Visser, H. G. & Steyl, G. (2007). Acta Cryst. E63, m3195-m3196.]); Wang et al. (2003[Wang, W., Spingler, B. & Alberto, R. (2003). Inorg. Chim. Acta, 355, 386-391.]); Alvarez et al. (2007[Alvarez, C. M., Garcia-Rodriguez, R. & Miguel, D. (2007). Dalton Trans. pp. 3546-3554.]). For the synthesis of the precursor, see: Alberto et al. (1996[Alberto, R., Schibli, R. & Schubiger, P. A. (1996). Polyhedron, 15, 1079-1083.]);

[Scheme 1]

Experimental

Crystal data
  • [Re(C7H4NO4)(CO)3(H2O)]

  • Mr = 454.37

  • Triclinic, [P \overline 1]

  • a = 9.5024 (11) Å

  • b = 12.4254 (16) Å

  • c = 12.4889 (16) Å

  • α = 101.799 (4)°

  • β = 107.943 (4)°

  • γ = 111.346 (4)°

  • V = 1220.4 (3) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 10.00 mm−1

  • T = 100 (2) K

  • 0.27 × 0.17 × 0.05 mm

Data collection
  • Bruker APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.140, Tmax = 0.605

  • 15096 measured reflections

  • 5848 independent reflections

  • 4869 reflections with I > 2σ(I)

  • Rint = 0.037

Refinement
  • R[F2 > 2σ(F2)] = 0.026

  • wR(F2) = 0.065

  • S = 1.05

  • 5848 reflections

  • 373 parameters

  • 7 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 1.21 e Å−3

  • Δρmin = −1.80 e Å−3

Table 1
Selected geometric parameters (Å, °)

N1—Re1 2.180 (4)
O5—Re1 2.153 (3)
O15—Re2 2.148 (3)
N2—Re2 2.166 (4)
C11—Re2 1.892 (5)
C12—Re2 1.947 (5)
C2—Re1 1.906 (5)
C3—Re1 1.885 (6)
C13—Re2 1.883 (5)
O14—Re2 2.153 (3)
O4—Re1 2.170 (3)
Re1—C1 1.915 (5)
C11—Re2—C12 89.52 (19)
C11—Re2—O15 170.52 (16)
C12—Re2—O15 98.45 (16)
C11—Re2—O14 95.63 (16)
C12—Re2—O14 96.35 (17)
O15—Re2—O14 78.48 (12)
O15—Re2—N2 74.98 (12)
C2—Re1—O5 98.77 (15)
C1—Re1—O4 95.49 (17)
O5—Re1—O4 80.73 (12)
O5—Re1—N1 74.77 (12)

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O7—H7⋯O15i 0.82 1.81 2.595 (4) 160
O4—H4B⋯O16ii 0.85 (5) 2.51 (5) 2.920 (5) 111 (4)
O4—H4B⋯O8iii 0.85 (5) 2.01 (3) 2.780 (5) 150 (5)
O4—H4B⋯O16ii 0.85 (5) 2.51 (5) 2.920 (5) 111 (4)
O14—H14B⋯O6 0.85 (5) 1.84 (2) 2.671 (5) 169 (5)
O14—H14A⋯O18iii 0.840 (18) 1.87 (2) 2.674 (4) 161 (5)
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z+1; (iii) x-1, y, z.

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2004[Bruker (2004). SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenberg & Putz, 2005[Brandenberg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and ORTEP-3 (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

The title compound, Re(C10H6NO8),is one of many Re(I)-tricarbonyl complexes currently under investigation in the field of radiopharmacology. One polymorph of the title compound was reported earlier [Mundwiler et al., (2004)].

The Re(I) core is coordinated by three facial carbonyl groups, one pyridine-2-carboxylato-4-carboxylic acid ligand and a water molecule. A slightly distorted octahedral geometry around the Re(I) metal centre is observed, possibly due to the effect of the small bite angles of 74.78 (14)° and 74.98 (12)° respectively for the two pyridine-2,4-dicarboxylic acid units. The Re—OH2 bond distances of 2.153 (4) Å and 2.170 (4) Å compare well with related structures [Mundwiler et al., (2004) and Kemp, (2006)] of 2.198 (5) Å and 2.192 (4) Å. The Re—CO distances are well within the normal range, 1.883 (6) Å to 1.947 (6) Å. The crystal structure shows a range of hydrogen bonding of the types OH—O and CH—O thereby forming a 3D polymeric network, with DA distances ranging from 2.595 (4) Å to 3.426 (5) Å.

Related literature top

For the monoclinic polymorph of the title compound, see: Mundwiler et al. (2004). For related structures, see: Kemp (2006); Roodt et al. (2003); Schutte et al. (2007); Wang et al. (2003); Alvarez et al. (2007). For the synthesis of the precursor, see: Alberto et al. (1996);

Experimental top

[NEt4]2[Re(CO)3Br3] (300 mg, 0.389 mmol), as prepared by Alberto et al. (1996) was stirred in 40 ml of water at pH 2.2 for 20 minutes until dissolved. AgNO3 (198 mg, 1.167 mmol) was added to the solution and stirred for 24 h at room temperature. The precipitate, AgBr, was filtered off and weighed(0.220 g). 2,4-Pyridinedicarboxylic acid (65 mg, 0.389 mmol) was added to the filtrate as a solid and stirred for 36 h. The solution turned bright yellow with a light yellow precipitate. The product was filtered off, dried and weighed. Crystals were obtained by slow evaporation of the filtrate. (Yield: 0.240 g, 68%).

Refinement top

The aromatic H atoms were placed in geometrically idealized positions and constrained to ride on its parent atoms with U<i/>iso(H) = 1.2U<i/>eq(C). The highest electron density lies within 1.14 Å from Re1. The hydrogen atoms of the coordinated water molecules were determined from a difference Fourier map and their positional parameters freely refined with U<i/>iso(H) = 1.5U<i/>eq(O).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenberg & Putz, 2005) and ORTEP-3 (Farrugia, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Representation of the title compound, showing the numbering scheme and displacement ellipsoids (50% probability).
Aquatricarbonyl(4-carboxypyridine-2-carboxylato- κ2N,O2)rhenium(I) top
Crystal data top
[Re(C7H4NO4)(CO)3(H2O)]Z = 4
Mr = 454.37F(000) = 848.0
Triclinic, P1Dx = 2.473 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.5024 (11) ÅCell parameters from 7140 reflections
b = 12.4254 (16) Åθ = 2.8–28.3°
c = 12.4889 (16) ŵ = 10.00 mm1
α = 101.799 (4)°T = 100 K
β = 107.943 (4)°Plate, yellow
γ = 111.346 (4)°0.27 × 0.17 × 0.05 mm
V = 1220.4 (3) Å3
Data collection top
Bruker APEX
diffractometer
4869 reflections with I > 2σ(I)
ϕ and ω scansRint = 0.037
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
θmax = 28.3°, θmin = 1.8°
Tmin = 0.140, Tmax = 0.605h = 1212
15096 measured reflectionsk = 1615
5048 independent reflectionsl = 1616
Refinement top
Refinement on F27 restraints
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.027 w = 1/[σ2(Fo2) + (0.0251P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.065(Δ/σ)max = 0.015
S = 1.05Δρmax = 1.21 e Å3
5848 reflectionsΔρmin = 1.80 e Å3
373 parameters
Crystal data top
[Re(C7H4NO4)(CO)3(H2O)]γ = 111.346 (4)°
Mr = 454.37V = 1220.4 (3) Å3
Triclinic, P1Z = 4
a = 9.5024 (11) ÅMo Kα radiation
b = 12.4254 (16) ŵ = 10.00 mm1
c = 12.4889 (16) ÅT = 100 K
α = 101.799 (4)°0.27 × 0.17 × 0.05 mm
β = 107.943 (4)°
Data collection top
Bruker APEX
diffractometer
5048 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
4869 reflections with I > 2σ(I)
Tmin = 0.140, Tmax = 0.605Rint = 0.037
15096 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0277 restraints
wR(F2) = 0.065H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 1.21 e Å3
5848 reflectionsΔρmin = 1.80 e Å3
373 parameters
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
N10.3078 (4)0.2654 (3)0.5400 (3)0.0095 (8)
O50.1030 (4)0.1933 (3)0.3130 (2)0.0113 (7)
O60.2391 (4)0.1072 (3)0.2433 (3)0.0152 (7)
C40.2193 (6)0.1635 (4)0.3289 (4)0.0116 (9)
O150.0841 (4)0.2152 (3)0.1450 (3)0.0112 (7)
C50.3392 (6)0.1998 (4)0.4572 (4)0.0102 (9)
O160.0735 (4)0.0827 (3)0.3002 (3)0.0160 (7)
C150.3019 (5)0.1585 (4)0.1099 (4)0.0097 (9)
C140.1407 (6)0.1487 (4)0.1934 (4)0.0118 (10)
C180.5968 (5)0.1949 (4)0.0518 (4)0.0116 (9)
H180.69810.20890.10840.014*
C170.5336 (6)0.1168 (4)0.0662 (4)0.0115 (9)
C160.3816 (5)0.0981 (4)0.1491 (4)0.0106 (9)
H160.33580.04590.22880.013*
C80.5409 (6)0.2756 (4)0.6944 (4)0.0127 (10)
H80.60810.30190.77610.015*
C60.4696 (6)0.1716 (4)0.4875 (4)0.0129 (10)
H60.48840.12780.42820.015*
C90.4082 (5)0.3013 (4)0.6568 (4)0.0122 (10)
H90.38740.34530.71460.015*
C70.5727 (5)0.2098 (4)0.6085 (4)0.0105 (9)
C200.6310 (6)0.0551 (4)0.0994 (4)0.0131 (10)
C190.5084 (5)0.2516 (4)0.0845 (4)0.0118 (10)
H190.55070.30310.16410.014*
N20.3633 (4)0.2346 (3)0.0051 (3)0.0092 (8)
O80.7441 (4)0.1233 (3)0.5666 (3)0.0200 (8)
O70.8100 (4)0.2290 (3)0.7589 (3)0.0190 (8)
H70.88780.21180.7730.029*
C100.7178 (5)0.1827 (4)0.6423 (4)0.0134 (10)
O180.7570 (4)0.0669 (3)0.0231 (3)0.0174 (8)
O170.5674 (4)0.0113 (3)0.2139 (3)0.0176 (8)
H170.62640.04240.22580.026*
O110.4169 (4)0.4220 (3)0.3181 (3)0.0206 (8)
O120.0486 (5)0.3985 (3)0.0753 (3)0.0290 (9)
C110.3339 (6)0.3833 (4)0.2154 (4)0.0129 (10)
C120.0473 (6)0.3683 (4)0.0652 (4)0.0165 (10)
O20.2361 (5)0.3030 (4)0.3410 (3)0.0296 (10)
C20.1119 (6)0.3005 (4)0.3895 (4)0.0178 (11)
C30.2069 (6)0.4532 (5)0.4629 (4)0.0211 (12)
O30.2698 (5)0.5484 (3)0.4535 (3)0.0283 (9)
C130.3283 (6)0.4712 (5)0.0407 (4)0.0162 (10)
O130.4026 (4)0.5690 (3)0.0395 (3)0.0209 (8)
O140.0791 (4)0.1290 (3)0.0380 (3)0.0128 (7)
O40.0362 (4)0.1106 (3)0.4661 (3)0.0191 (8)
H4A0.070 (6)0.046 (3)0.408 (3)0.029*
H4B0.092 (6)0.097 (4)0.508 (4)0.029*
H14B0.123 (5)0.112 (5)0.098 (3)0.029*
H14A0.025 (2)0.093 (4)0.010 (4)0.029*
Re20.20999 (2)0.315032 (16)0.046124 (15)0.00973 (6)
Re10.09158 (2)0.296297 (16)0.468442 (15)0.01020 (6)
C10.1002 (6)0.3789 (5)0.6194 (4)0.0165 (10)
O10.1138 (5)0.4303 (3)0.7126 (3)0.0272 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
N10.0096 (18)0.013 (2)0.0088 (18)0.0082 (16)0.0031 (15)0.0057 (16)
O50.0128 (16)0.0157 (18)0.0070 (15)0.0087 (14)0.0052 (13)0.0014 (13)
O60.0183 (17)0.0185 (19)0.0109 (16)0.0125 (15)0.0057 (14)0.0022 (14)
C40.016 (2)0.013 (2)0.013 (2)0.010 (2)0.0097 (19)0.0047 (19)
O150.0142 (16)0.0144 (17)0.0063 (14)0.0101 (14)0.0035 (13)0.0007 (13)
C50.012 (2)0.008 (2)0.006 (2)0.0038 (18)0.0014 (17)0.0007 (17)
O160.0185 (18)0.0204 (19)0.0076 (15)0.0131 (15)0.0024 (13)0.0010 (14)
C150.012 (2)0.008 (2)0.009 (2)0.0047 (18)0.0040 (18)0.0034 (18)
C140.012 (2)0.016 (3)0.010 (2)0.008 (2)0.0044 (18)0.0060 (19)
C180.006 (2)0.017 (3)0.009 (2)0.0058 (19)0.0008 (17)0.0032 (19)
C170.015 (2)0.011 (2)0.014 (2)0.0092 (19)0.0085 (19)0.0059 (19)
C160.011 (2)0.010 (2)0.008 (2)0.0039 (19)0.0039 (17)0.0016 (18)
C80.012 (2)0.016 (2)0.006 (2)0.006 (2)0.0017 (17)0.0023 (18)
C60.013 (2)0.010 (2)0.013 (2)0.0028 (19)0.0073 (19)0.0026 (19)
C90.013 (2)0.015 (2)0.006 (2)0.008 (2)0.0025 (18)0.0010 (18)
C70.005 (2)0.014 (2)0.011 (2)0.0053 (18)0.0015 (17)0.0029 (19)
C200.012 (2)0.014 (2)0.016 (2)0.008 (2)0.0073 (19)0.005 (2)
C190.010 (2)0.014 (2)0.008 (2)0.0056 (19)0.0030 (18)0.0001 (18)
N20.0081 (18)0.010 (2)0.0085 (18)0.0053 (16)0.0021 (14)0.0014 (15)
O80.0175 (18)0.027 (2)0.0152 (17)0.0143 (16)0.0046 (14)0.0022 (15)
O70.0150 (17)0.029 (2)0.0117 (16)0.0145 (16)0.0008 (14)0.0025 (15)
C100.006 (2)0.017 (3)0.016 (2)0.0058 (19)0.0029 (18)0.006 (2)
O180.0116 (17)0.026 (2)0.0170 (17)0.0135 (16)0.0056 (14)0.0040 (15)
O170.0187 (18)0.025 (2)0.0133 (17)0.0179 (16)0.0065 (14)0.0014 (15)
O110.0230 (19)0.021 (2)0.0082 (16)0.0068 (16)0.0034 (14)0.0011 (15)
O120.028 (2)0.028 (2)0.041 (2)0.0201 (19)0.0204 (19)0.0099 (19)
C110.013 (2)0.012 (2)0.019 (2)0.009 (2)0.0114 (19)0.005 (2)
C120.018 (3)0.011 (2)0.018 (2)0.006 (2)0.007 (2)0.002 (2)
O20.026 (2)0.044 (3)0.0178 (18)0.027 (2)0.0004 (16)0.0021 (18)
C20.026 (3)0.019 (3)0.010 (2)0.012 (2)0.010 (2)0.002 (2)
C30.022 (3)0.020 (3)0.018 (3)0.012 (2)0.007 (2)0.002 (2)
O30.040 (2)0.020 (2)0.033 (2)0.0141 (19)0.0231 (19)0.0118 (18)
C130.018 (2)0.016 (3)0.012 (2)0.010 (2)0.0043 (19)0.000 (2)
O130.029 (2)0.0149 (19)0.0237 (19)0.0093 (16)0.0168 (16)0.0079 (15)
O140.0086 (16)0.0141 (18)0.0141 (17)0.0046 (14)0.0031 (13)0.0054 (14)
O40.025 (2)0.0138 (19)0.0214 (19)0.0088 (16)0.0164 (16)0.0019 (15)
Re20.00971 (10)0.01041 (10)0.00854 (9)0.00554 (8)0.00342 (7)0.00128 (7)
Re10.01226 (10)0.01220 (11)0.00847 (9)0.00860 (8)0.00437 (7)0.00248 (8)
C10.016 (2)0.017 (3)0.023 (3)0.011 (2)0.009 (2)0.012 (2)
O10.039 (2)0.028 (2)0.0169 (19)0.0175 (19)0.0158 (17)0.0020 (17)
Geometric parameters (Å, º) top
N1—C91.343 (5)C7—C101.493 (6)
N1—C51.357 (5)C20—O181.215 (5)
N1—Re12.180 (4)C20—O171.309 (5)
O5—C41.261 (5)C19—N21.337 (5)
O5—Re12.153 (3)C19—H190.93
O6—C41.258 (5)N2—Re22.166 (4)
C4—O61.258 (5)O8—C101.223 (5)
C4—C51.508 (6)O7—C101.313 (5)
O15—C141.287 (5)O11—C111.161 (5)
O15—Re22.148 (3)O12—C121.135 (6)
C5—C61.372 (6)C11—Re21.892 (5)
O16—C141.227 (5)C12—Re21.947 (5)
C15—N21.351 (5)O2—C21.164 (6)
C15—C161.368 (6)C2—Re11.906 (5)
C15—C141.508 (6)C3—O31.165 (6)
C18—C191.376 (6)C3—Re11.885 (6)
C18—C171.385 (6)C13—O131.169 (6)
C18—H180.93C13—Re21.883 (5)
C17—C161.395 (6)O14—Re22.153 (3)
C17—C201.496 (6)O14—H14B0.85 (4)
C16—H160.93O14—H14A0.85 (4)
C8—C91.379 (6)O4—Re12.170 (3)
C8—C71.390 (6)O4—H4A0.85 (5)
C8—H80.93O4—H4B0.85 (5)
C6—C71.388 (6)Re1—C11.915 (5)
C6—H60.93C1—O11.151 (5)
C9—H90.93
C9—N1—C5117.6 (4)C15—N2—Re2115.9 (3)
C9—N1—Re1126.4 (3)C10—O7—H7109.5
C5—N1—Re1115.9 (3)O8—C10—O7125.2 (4)
C4—O5—Re1118.5 (3)O8—C10—C7121.8 (4)
O6—C4—O5122.9 (4)O7—C10—C7113.0 (4)
O6—C4—O5122.9 (4)C20—O17—H17109.5
O6—C4—C5119.9 (4)O11—C11—Re2175.5 (4)
O6—C4—C5119.9 (4)O12—C12—Re2179.4 (5)
O5—C4—C5117.2 (4)O2—C2—Re1179.9 (5)
C14—O15—Re2118.6 (3)O3—C3—Re1176.0 (5)
N1—C5—C6123.1 (4)O13—C13—Re2178.8 (4)
N1—C5—C4113.5 (4)Re2—O14—H14B116 (3)
C6—C5—C4123.3 (4)Re2—O14—H14A121 (3)
N2—C15—C16122.9 (4)H14B—O14—H14A112 (3)
N2—C15—C14114.7 (4)Re1—O4—H4A124 (3)
C16—C15—C14122.3 (4)Re1—O4—H4B121 (3)
O16—C14—O15124.0 (4)H4A—O4—H4B110 (3)
O16—C14—C15120.6 (4)C13—Re2—C1188.2 (2)
O15—C14—C15115.4 (4)C13—Re2—C1287.6 (2)
C19—C18—C17119.4 (4)C11—Re2—C1289.52 (19)
C19—C18—H18120.3C13—Re2—O1597.19 (16)
C17—C18—H18120.3C11—Re2—O15170.52 (16)
C18—C17—C16118.9 (4)C12—Re2—O1598.45 (16)
C18—C17—C20118.5 (4)C13—Re2—O14174.48 (16)
C16—C17—C20122.6 (4)C11—Re2—O1495.63 (16)
C15—C16—C17118.2 (4)C12—Re2—O1496.35 (17)
C15—C16—H16120.9O15—Re2—O1478.48 (12)
C17—C16—H16120.9C13—Re2—N296.92 (17)
C9—C8—C7119.0 (4)C11—Re2—N296.70 (16)
C9—C8—H8120.5C12—Re2—N2172.39 (16)
C7—C8—H8120.5O15—Re2—N274.98 (12)
C5—C6—C7118.6 (4)O14—Re2—N278.73 (13)
C5—C6—H6120.7C3—Re1—C288.6 (2)
C7—C6—H6120.7C3—Re1—C188.1 (2)
N1—C9—C8122.7 (4)C2—Re1—C188.6 (2)
N1—C9—H9118.7C3—Re1—O595.56 (17)
C8—C9—H9118.7C2—Re1—O598.77 (15)
C6—C7—C8119.0 (4)C1—Re1—O5171.85 (16)
C6—C7—C10119.0 (4)C3—Re1—O4176.21 (16)
C8—C7—C10122.0 (4)C2—Re1—O492.71 (18)
O18—C20—O17124.8 (4)C1—Re1—O495.49 (17)
O18—C20—C17120.7 (4)O5—Re1—O480.73 (12)
O17—C20—C17114.5 (4)C3—Re1—N196.75 (18)
N2—C19—C18121.8 (4)C2—Re1—N1171.93 (16)
N2—C19—H19119.1C1—Re1—N197.60 (17)
C18—C19—H19119.1O5—Re1—N174.77 (12)
C19—N2—C15118.7 (4)O4—Re1—N181.58 (14)
C19—N2—Re2125.3 (3)O1—C1—Re1176.6 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7···O15i0.821.812.595 (4)160
O4—H4B···O16ii0.85 (5)2.51 (5)2.920 (5)111 (4)
O4—H4B···O8iii0.85 (5)2.01 (3)2.780 (5)150 (5)
O4—H4B···O16ii0.85 (5)2.51 (5)2.920 (5)111 (4)
O14—H14B···O60.85 (5)1.84 (2)2.671 (5)169 (5)
O14—H14A···O18iii0.84 (2)1.87 (2)2.674 (4)161 (5)
O17—H17···O6iv0.821.782.602 (4)177
C8—H8···O13v0.932.583.253 (5)130
C6—H6···O17iv0.932.553.426 (5)156
C19—H19···O2vi0.932.53.131 (5)126
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z+1; (iii) x1, y, z; (iv) x+1, y, z; (v) x+1, y+1, z+1; (vi) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Re(C7H4NO4)(CO)3(H2O)]
Mr454.37
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)9.5024 (11), 12.4254 (16), 12.4889 (16)
α, β, γ (°)101.799 (4), 107.943 (4), 111.346 (4)
V3)1220.4 (3)
Z4
Radiation typeMo Kα
µ (mm1)10.00
Crystal size (mm)0.27 × 0.17 × 0.05
Data collection
DiffractometerBruker APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2004)
Tmin, Tmax0.140, 0.605
No. of measured, independent and
observed [I > 2σ(I)] reflections
15096, 5048, 4869
Rint0.037
(sin θ/λ)max1)0.668
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.065, 1.05
No. of reflections5848
No. of parameters373
No. of restraints7
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.21, 1.80

Computer programs: APEX2 (Bruker, 2005), SAINT-Plus (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenberg & Putz, 2005) and ORTEP-3 (Farrugia, 1999).

Selected geometric parameters (Å, º) top
N1—Re12.180 (4)C2—Re11.906 (5)
O5—Re12.153 (3)C3—Re11.885 (6)
O15—Re22.148 (3)C13—Re21.883 (5)
N2—Re22.166 (4)O14—Re22.153 (3)
C11—Re21.892 (5)O4—Re12.170 (3)
C12—Re21.947 (5)Re1—C11.915 (5)
C11—Re2—C1289.52 (19)O15—Re2—N274.98 (12)
C11—Re2—O15170.52 (16)C2—Re1—O598.77 (15)
C12—Re2—O1598.45 (16)C1—Re1—O495.49 (17)
C11—Re2—O1495.63 (16)O5—Re1—O480.73 (12)
C12—Re2—O1496.35 (17)O5—Re1—N174.77 (12)
O15—Re2—O1478.48 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7···O15i0.821.812.595 (4)159.7
O4—H4B···O16ii0.85 (5)2.51 (5)2.920 (5)111 (4)
O4—H4B···O8iii0.85 (5)2.01 (3)2.780 (5)150 (5)
O4—H4B···O16ii0.85 (5)2.51 (5)2.920 (5)111 (4)
O14—H14B···O60.85 (5)1.84 (2)2.671 (5)169 (5)
O14—H14A···O18iii0.840 (18)1.87 (2)2.674 (4)161 (5)
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z+1; (iii) x1, y, z.
 

Acknowledgements

The University of the Free State and Professor A. Roodt are gratefully aknowledged for financial support. Dr A.J. Muller is kindly acknowledged for the data collection.

References

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Volume 64| Part 10| October 2008| Pages m1226-m1227
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