Aqua-tricarbon-yl(4-carboxy-pyridine-2-carboxyl-ato-κN,O)rhenium(I).

There are two mol-ecules with similar bond dimensions in the asymmetric unit of the title complex, [Re(C(7)H(4)NO(4))(CO)(3)(H(2)O)]. The metal centre is coordinated facially by three carbonyl groups, is chelated by a 4-carboxy-pyridine-2-carboxyl-ate ligand and is also coordinated by a water mol-ecule. 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 ▶). 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

Crystal data

[Re(C7H4NO4)(CO)3(H2O)]

M = 454.37

Triclinic,

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 ▶) T min = 0.140, T max = 0.605

15096 measured reflections

5848 independent reflections

4869 reflections with I > 2σ(I)

R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.026

wR(F 2) = 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

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: SAINT-Plus (Bruker, 2004 ▶); data reduction: SAINT-Plus; 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.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680802761X/ng2479sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680802761X/ng2479Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Re(C7H4NO4)(CO)3(H2O)]	Z = 4
Mr = 454.37	F(000) = 848.0
Triclinic, P1	Dx = 2.473 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.5024 (11) Å	Cell parameters from 7140 reflections
b = 12.4254 (16) Å	θ = 2.8–28.3°
c = 12.4889 (16) Å	µ = 10.00 mm−1
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

Bruker APEX diffractometer	4869 reflections with I > 2σ(I)
φ and ω scans	Rint = 0.037
Absorption correction: multi-scan (SADABS; Bruker, 2004)	θmax = 28.3°, θmin = 1.8°
Tmin = 0.140, Tmax = 0.605	h = −12→12
15096 measured reflections	k = −16→15
5048 independent reflections	l = −16→16

Refinement on F2	7 restraints
Least-squares matrix: full	H 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 = 1.05	Δρmax = 1.21 e Å−3
5848 reflections	Δρmin = −1.80 e Å−3
373 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.

	x	y	z	Uiso*/Ueq
N1	0.3078 (4)	0.2654 (3)	0.5400 (3)	0.0095 (8)
O5	0.1030 (4)	0.1933 (3)	0.3130 (2)	0.0113 (7)
O6	0.2391 (4)	0.1072 (3)	0.2433 (3)	0.0152 (7)
C4	0.2193 (6)	0.1635 (4)	0.3289 (4)	0.0116 (9)
O15	0.0841 (4)	0.2152 (3)	−0.1450 (3)	0.0112 (7)
C5	0.3392 (6)	0.1998 (4)	0.4572 (4)	0.0102 (9)
O16	0.0735 (4)	0.0827 (3)	−0.3002 (3)	0.0160 (7)
C15	0.3019 (5)	0.1585 (4)	−0.1099 (4)	0.0097 (9)
C14	0.1407 (6)	0.1487 (4)	−0.1934 (4)	0.0118 (10)
C18	0.5968 (5)	0.1949 (4)	0.0518 (4)	0.0116 (9)
H18	0.6981	0.2089	0.1084	0.014*
C17	0.5336 (6)	0.1168 (4)	−0.0662 (4)	0.0115 (9)
C16	0.3816 (5)	0.0981 (4)	−0.1491 (4)	0.0106 (9)
H16	0.3358	0.0459	−0.2288	0.013*
C8	0.5409 (6)	0.2756 (4)	0.6944 (4)	0.0127 (10)
H8	0.6081	0.3019	0.7761	0.015*
C6	0.4696 (6)	0.1716 (4)	0.4875 (4)	0.0129 (10)
H6	0.4884	0.1278	0.4282	0.015*
C9	0.4082 (5)	0.3013 (4)	0.6568 (4)	0.0122 (10)
H9	0.3874	0.3453	0.7146	0.015*
C7	0.5727 (5)	0.2098 (4)	0.6085 (4)	0.0105 (9)
C20	0.6310 (6)	0.0551 (4)	−0.0994 (4)	0.0131 (10)
C19	0.5084 (5)	0.2516 (4)	0.0845 (4)	0.0118 (10)
H19	0.5507	0.3031	0.1641	0.014*
N2	0.3633 (4)	0.2346 (3)	0.0051 (3)	0.0092 (8)
O8	0.7441 (4)	0.1233 (3)	0.5666 (3)	0.0200 (8)
O7	0.8100 (4)	0.2290 (3)	0.7589 (3)	0.0190 (8)
H7	0.8878	0.2118	0.773	0.029*
C10	0.7178 (5)	0.1827 (4)	0.6423 (4)	0.0134 (10)
O18	0.7570 (4)	0.0669 (3)	−0.0231 (3)	0.0174 (8)
O17	0.5674 (4)	−0.0113 (3)	−0.2139 (3)	0.0176 (8)
H17	0.6264	−0.0424	−0.2258	0.026*
O11	0.4169 (4)	0.4220 (3)	0.3181 (3)	0.0206 (8)
O12	−0.0486 (5)	0.3985 (3)	0.0753 (3)	0.0290 (9)
C11	0.3339 (6)	0.3833 (4)	0.2154 (4)	0.0129 (10)
C12	0.0473 (6)	0.3683 (4)	0.0652 (4)	0.0165 (10)
O2	−0.2361 (5)	0.3030 (4)	0.3410 (3)	0.0296 (10)
C2	−0.1119 (6)	0.3005 (4)	0.3895 (4)	0.0178 (11)
C3	0.2069 (6)	0.4532 (5)	0.4629 (4)	0.0211 (12)
O3	0.2698 (5)	0.5484 (3)	0.4535 (3)	0.0283 (9)
C13	0.3283 (6)	0.4712 (5)	0.0407 (4)	0.0162 (10)
O13	0.4026 (4)	0.5690 (3)	0.0395 (3)	0.0209 (8)
O14	0.0791 (4)	0.1290 (3)	0.0380 (3)	0.0128 (7)
O4	−0.0362 (4)	0.1106 (3)	0.4661 (3)	0.0191 (8)
H4A	−0.070 (6)	0.046 (3)	0.408 (3)	0.029*
H4B	−0.092 (6)	0.097 (4)	0.508 (4)	0.029*
H14B	0.123 (5)	0.112 (5)	0.098 (3)	0.029*
H14A	−0.025 (2)	0.093 (4)	0.010 (4)	0.029*
Re2	0.20999 (2)	0.315032 (16)	0.046124 (15)	0.00973 (6)
Re1	0.09158 (2)	0.296297 (16)	0.468442 (15)	0.01020 (6)
C1	0.1002 (6)	0.3789 (5)	0.6194 (4)	0.0165 (10)
O1	0.1138 (5)	0.4303 (3)	0.7126 (3)	0.0272 (9)

	U11	U22	U33	U12	U13	U23
N1	0.0096 (18)	0.013 (2)	0.0088 (18)	0.0082 (16)	0.0031 (15)	0.0057 (16)
O5	0.0128 (16)	0.0157 (18)	0.0070 (15)	0.0087 (14)	0.0052 (13)	0.0014 (13)
O6	0.0183 (17)	0.0185 (19)	0.0109 (16)	0.0125 (15)	0.0057 (14)	0.0022 (14)
C4	0.016 (2)	0.013 (2)	0.013 (2)	0.010 (2)	0.0097 (19)	0.0047 (19)
O15	0.0142 (16)	0.0144 (17)	0.0063 (14)	0.0101 (14)	0.0035 (13)	0.0007 (13)
C5	0.012 (2)	0.008 (2)	0.006 (2)	0.0038 (18)	0.0014 (17)	−0.0007 (17)
O16	0.0185 (18)	0.0204 (19)	0.0076 (15)	0.0131 (15)	0.0024 (13)	−0.0010 (14)
C15	0.012 (2)	0.008 (2)	0.009 (2)	0.0047 (18)	0.0040 (18)	0.0034 (18)
C14	0.012 (2)	0.016 (3)	0.010 (2)	0.008 (2)	0.0044 (18)	0.0060 (19)
C18	0.006 (2)	0.017 (3)	0.009 (2)	0.0058 (19)	0.0008 (17)	0.0032 (19)
C17	0.015 (2)	0.011 (2)	0.014 (2)	0.0092 (19)	0.0085 (19)	0.0059 (19)
C16	0.011 (2)	0.010 (2)	0.008 (2)	0.0039 (19)	0.0039 (17)	0.0016 (18)
C8	0.012 (2)	0.016 (2)	0.006 (2)	0.006 (2)	0.0017 (17)	0.0023 (18)
C6	0.013 (2)	0.010 (2)	0.013 (2)	0.0028 (19)	0.0073 (19)	0.0026 (19)
C9	0.013 (2)	0.015 (2)	0.006 (2)	0.008 (2)	0.0025 (18)	−0.0010 (18)
C7	0.005 (2)	0.014 (2)	0.011 (2)	0.0053 (18)	0.0015 (17)	0.0029 (19)
C20	0.012 (2)	0.014 (2)	0.016 (2)	0.008 (2)	0.0073 (19)	0.005 (2)
C19	0.010 (2)	0.014 (2)	0.008 (2)	0.0056 (19)	0.0030 (18)	0.0001 (18)
N2	0.0081 (18)	0.010 (2)	0.0085 (18)	0.0053 (16)	0.0021 (14)	0.0014 (15)
O8	0.0175 (18)	0.027 (2)	0.0152 (17)	0.0143 (16)	0.0046 (14)	0.0022 (15)
O7	0.0150 (17)	0.029 (2)	0.0117 (16)	0.0145 (16)	0.0008 (14)	0.0025 (15)
C10	0.006 (2)	0.017 (3)	0.016 (2)	0.0058 (19)	0.0029 (18)	0.006 (2)
O18	0.0116 (17)	0.026 (2)	0.0170 (17)	0.0135 (16)	0.0056 (14)	0.0040 (15)
O17	0.0187 (18)	0.025 (2)	0.0133 (17)	0.0179 (16)	0.0065 (14)	0.0014 (15)
O11	0.0230 (19)	0.021 (2)	0.0082 (16)	0.0068 (16)	0.0034 (14)	−0.0011 (15)
O12	0.028 (2)	0.028 (2)	0.041 (2)	0.0201 (19)	0.0204 (19)	0.0099 (19)
C11	0.013 (2)	0.012 (2)	0.019 (2)	0.009 (2)	0.0114 (19)	0.005 (2)
C12	0.018 (3)	0.011 (2)	0.018 (2)	0.006 (2)	0.007 (2)	0.002 (2)
O2	0.026 (2)	0.044 (3)	0.0178 (18)	0.027 (2)	0.0004 (16)	0.0021 (18)
C2	0.026 (3)	0.019 (3)	0.010 (2)	0.012 (2)	0.010 (2)	0.002 (2)
C3	0.022 (3)	0.020 (3)	0.018 (3)	0.012 (2)	0.007 (2)	−0.002 (2)
O3	0.040 (2)	0.020 (2)	0.033 (2)	0.0141 (19)	0.0231 (19)	0.0118 (18)
C13	0.018 (2)	0.016 (3)	0.012 (2)	0.010 (2)	0.0043 (19)	0.000 (2)
O13	0.029 (2)	0.0149 (19)	0.0237 (19)	0.0093 (16)	0.0168 (16)	0.0079 (15)
O14	0.0086 (16)	0.0141 (18)	0.0141 (17)	0.0046 (14)	0.0031 (13)	0.0054 (14)
O4	0.025 (2)	0.0138 (19)	0.0214 (19)	0.0088 (16)	0.0164 (16)	0.0019 (15)
Re2	0.00971 (10)	0.01041 (10)	0.00854 (9)	0.00554 (8)	0.00342 (7)	0.00128 (7)
Re1	0.01226 (10)	0.01220 (11)	0.00847 (9)	0.00860 (8)	0.00437 (7)	0.00248 (8)
C1	0.016 (2)	0.017 (3)	0.023 (3)	0.011 (2)	0.009 (2)	0.012 (2)
O1	0.039 (2)	0.028 (2)	0.0169 (19)	0.0175 (19)	0.0158 (17)	0.0020 (17)

N1—C9	1.343 (5)	C7—C10	1.493 (6)
N1—C5	1.357 (5)	C20—O18	1.215 (5)
N1—Re1	2.180 (4)	C20—O17	1.309 (5)
O5—C4	1.261 (5)	C19—N2	1.337 (5)
O5—Re1	2.153 (3)	C19—H19	0.93
O6—C4	1.258 (5)	N2—Re2	2.166 (4)
C4—O6	1.258 (5)	O8—C10	1.223 (5)
C4—C5	1.508 (6)	O7—C10	1.313 (5)
O15—C14	1.287 (5)	O11—C11	1.161 (5)
O15—Re2	2.148 (3)	O12—C12	1.135 (6)
C5—C6	1.372 (6)	C11—Re2	1.892 (5)
O16—C14	1.227 (5)	C12—Re2	1.947 (5)
C15—N2	1.351 (5)	O2—C2	1.164 (6)
C15—C16	1.368 (6)	C2—Re1	1.906 (5)
C15—C14	1.508 (6)	C3—O3	1.165 (6)
C18—C19	1.376 (6)	C3—Re1	1.885 (6)
C18—C17	1.385 (6)	C13—O13	1.169 (6)
C18—H18	0.93	C13—Re2	1.883 (5)
C17—C16	1.395 (6)	O14—Re2	2.153 (3)
C17—C20	1.496 (6)	O14—H14B	0.85 (4)
C16—H16	0.93	O14—H14A	0.85 (4)
C8—C9	1.379 (6)	O4—Re1	2.170 (3)
C8—C7	1.390 (6)	O4—H4A	0.85 (5)
C8—H8	0.93	O4—H4B	0.85 (5)
C6—C7	1.388 (6)	Re1—C1	1.915 (5)
C6—H6	0.93	C1—O1	1.151 (5)
C9—H9	0.93
C9—N1—C5	117.6 (4)	C15—N2—Re2	115.9 (3)
C9—N1—Re1	126.4 (3)	C10—O7—H7	109.5
C5—N1—Re1	115.9 (3)	O8—C10—O7	125.2 (4)
C4—O5—Re1	118.5 (3)	O8—C10—C7	121.8 (4)
O6—C4—O5	122.9 (4)	O7—C10—C7	113.0 (4)
O6—C4—O5	122.9 (4)	C20—O17—H17	109.5
O6—C4—C5	119.9 (4)	O11—C11—Re2	175.5 (4)
O6—C4—C5	119.9 (4)	O12—C12—Re2	179.4 (5)
O5—C4—C5	117.2 (4)	O2—C2—Re1	179.9 (5)
C14—O15—Re2	118.6 (3)	O3—C3—Re1	176.0 (5)
N1—C5—C6	123.1 (4)	O13—C13—Re2	178.8 (4)
N1—C5—C4	113.5 (4)	Re2—O14—H14B	116 (3)
C6—C5—C4	123.3 (4)	Re2—O14—H14A	121 (3)
N2—C15—C16	122.9 (4)	H14B—O14—H14A	112 (3)
N2—C15—C14	114.7 (4)	Re1—O4—H4A	124 (3)
C16—C15—C14	122.3 (4)	Re1—O4—H4B	121 (3)
O16—C14—O15	124.0 (4)	H4A—O4—H4B	110 (3)
O16—C14—C15	120.6 (4)	C13—Re2—C11	88.2 (2)
O15—C14—C15	115.4 (4)	C13—Re2—C12	87.6 (2)
C19—C18—C17	119.4 (4)	C11—Re2—C12	89.52 (19)
C19—C18—H18	120.3	C13—Re2—O15	97.19 (16)
C17—C18—H18	120.3	C11—Re2—O15	170.52 (16)
C18—C17—C16	118.9 (4)	C12—Re2—O15	98.45 (16)
C18—C17—C20	118.5 (4)	C13—Re2—O14	174.48 (16)
C16—C17—C20	122.6 (4)	C11—Re2—O14	95.63 (16)
C15—C16—C17	118.2 (4)	C12—Re2—O14	96.35 (17)
C15—C16—H16	120.9	O15—Re2—O14	78.48 (12)
C17—C16—H16	120.9	C13—Re2—N2	96.92 (17)
C9—C8—C7	119.0 (4)	C11—Re2—N2	96.70 (16)
C9—C8—H8	120.5	C12—Re2—N2	172.39 (16)
C7—C8—H8	120.5	O15—Re2—N2	74.98 (12)
C5—C6—C7	118.6 (4)	O14—Re2—N2	78.73 (13)
C5—C6—H6	120.7	C3—Re1—C2	88.6 (2)
C7—C6—H6	120.7	C3—Re1—C1	88.1 (2)
N1—C9—C8	122.7 (4)	C2—Re1—C1	88.6 (2)
N1—C9—H9	118.7	C3—Re1—O5	95.56 (17)
C8—C9—H9	118.7	C2—Re1—O5	98.77 (15)
C6—C7—C8	119.0 (4)	C1—Re1—O5	171.85 (16)
C6—C7—C10	119.0 (4)	C3—Re1—O4	176.21 (16)
C8—C7—C10	122.0 (4)	C2—Re1—O4	92.71 (18)
O18—C20—O17	124.8 (4)	C1—Re1—O4	95.49 (17)
O18—C20—C17	120.7 (4)	O5—Re1—O4	80.73 (12)
O17—C20—C17	114.5 (4)	C3—Re1—N1	96.75 (18)
N2—C19—C18	121.8 (4)	C2—Re1—N1	171.93 (16)
N2—C19—H19	119.1	C1—Re1—N1	97.60 (17)
C18—C19—H19	119.1	O5—Re1—N1	74.77 (12)
C19—N2—C15	118.7 (4)	O4—Re1—N1	81.58 (14)
C19—N2—Re2	125.3 (3)	O1—C1—Re1	176.6 (4)

D—H···A	D—H	H···A	D···A	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	0.84 (2)	1.87 (2)	2.674 (4)	161 (5)
O17—H17···O6iv	0.82	1.78	2.602 (4)	177.
C8—H8···O13v	0.93	2.58	3.253 (5)	130.
C6—H6···O17iv	0.93	2.55	3.426 (5)	156.
C19—H19···O2vi	0.93	2.5	3.131 (5)	126.

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	D⋯A	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) ; (ii) ; (iii) .