Aqua-tricarbon-yl(3,5,7-tribromo-tropolonato)rhenium(I) methanol solvate.

The title complex, [Re(C(7)H(2)Br(3)O(2))(CO)(3)(H(2)O)]·CH(3)OH, crystallized as a neutral Re(I) compound and one methanol solvent mol-ecule in the asymmetric unit. The metal centre is coordinated facially by three carbonyl groups. The bidentate tribromo-tropolanate ligand and a water mol-ecule complete the distorted octahedral coordination around the central metal. Inter-molecular Br⋯O [3.226 (5) Å] and Br⋯Br [3.590 (2) Å] contacts are observed between adjacent mol-ecules. These contacts, together with an array of O-H⋯O, O-H⋯Br and C-H⋯O hydrogen bonds, complete a three-dimensional polymeric network formed between the methanol solvent and the complex.

Related literature

For a smiliar tribromo­tropolonato ReI structure, see: Schutte et al. (2007 ▶). For other related structures, see: Kemp (2006 ▶); Roodt et al. (2003 ▶); Wang et al. (2003 ▶); Alvarez et al. (2007 ▶); Brasey et al. (2004 ▶); Gibson et al. (1999 ▶); Bochkova et al. (1987 ▶); Cheng et al. (1988 ▶); Mundwiler et al. (2004 ▶). For the synthesis of the precursor, see: Alberto et al. (1996 ▶). For synthesis of the tribromo­tropolone ligand, see: Steyl & Roodt (2006 ▶).

Experimental

Crystal data

[Re(C7H2Br3O2)(CO)3(H2O)]·CH4O

M = 678.1

Triclinic,

a = 9.090 (5) Å

b = 9.379 (5) Å

c = 10.010 (5) Å

α = 109.569 (5)°

β = 94.285 (5)°

γ = 102.133 (5)°

V = 776.3 (7) Å3

Z = 2

Mo Kα radiation

μ = 15.58 mm−1

T = 100 (2) K

0.19 × 0.06 × 0.03 mm

Data collection

Bruker APEX diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2004 ▶) T min = 0.150, T max = 0.626

8673 measured reflections

3599 independent reflections

3018 reflections with I > 2σ(I)

R int = 0.035

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.079

S = 1.05

3599 reflections

207 parameters

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 2.40 e Å−3

Δρmin = −2.11 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: SHELXS97 (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/S1600536808038737/kj2103sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808038737/kj2103Isup2.hkl

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

[Re(C7H2Br3O2)(CO)3(H2O)]·CH4O	Z = 2
Mr = 678.1	F000 = 620
Triclinic, P1	Dx = 2.901 Mg m−3
Hall symbol: -P 1	Mo Kα radiation λ = 0.71073 Å
a = 9.090 (5) Å	Cell parameters from 3145 reflections
b = 9.379 (5) Å	θ = 2.2–28.2º
c = 10.010 (5) Å	µ = 15.58 mm−1
α = 109.569 (5)º	T = 100 (2) K
β = 94.285 (5)º	Plate, orange
γ = 102.133 (5)º	0.19 × 0.06 × 0.03 mm
V = 776.3 (7) Å3

Bruker APEX diffractometer	Rint = 0.035
φ and ω scans	θmax = 28.3º
Absorption correction: multi-scan(SADABS; Bruker, 2004)	θmin = 2.2º
Tmin = 0.150, Tmax = 0.626	h = −8→12
8673 measured reflections	k = −11→12
3599 independent reflections	l = −13→10
3018 reflections with I > 2σ(I)

Refinement on F2	H atoms treated by a mixture of independent and constrained refinement
Least-squares matrix: full	w = 1/[σ2(Fo2) + (0.0385P)2] where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.033	(Δ/σ)max < 0.001
wR(F2) = 0.079	Δρmax = 2.41 e Å−3
S = 1.05	Δρmin = −2.11 e Å−3
3599 reflections	Extinction correction: none
207 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
Re01	0.54228 (3)	0.51098 (3)	0.75340 (3)	0.00853 (8)
Br1	0.46576 (7)	0.05513 (7)	0.28520 (6)	0.01185 (14)
O4	0.3428 (5)	0.3587 (5)	0.7724 (4)	0.0107 (9)
C11	0.3852 (7)	0.1903 (7)	0.5557 (7)	0.0098 (13)
C2	0.7128 (8)	0.6389 (7)	0.7149 (7)	0.0141 (8)
C15	0.1120 (7)	−0.0432 (8)	0.6174 (7)	0.0130 (13)
H15	0.0347	−0.093	0.6543	0.016 (19)*
C3	0.5502 (8)	0.6908 (8)	0.9164 (7)	0.0141 (8)
C17	0.2988 (7)	0.2213 (7)	0.6772 (6)	0.0079 (12)
O5	0.4976 (5)	0.3042 (5)	0.5642 (4)	0.0096 (9)
C16	0.1735 (7)	0.1137 (7)	0.6939 (6)	0.0100 (13)
C12	0.3491 (7)	0.0514 (7)	0.4343 (6)	0.0084 (12)
C13	0.2524 (7)	−0.0921 (7)	0.4077 (7)	0.0101 (13)
H13	0.2554	−0.1698	0.3217	0.012 (18)*
C14	0.1514 (7)	−0.1368 (7)	0.4909 (7)	0.0135 (13)
Br2	0.04885 (8)	−0.35228 (8)	0.42285 (7)	0.01741 (15)
Br3	0.08290 (7)	0.19489 (8)	0.85829 (7)	0.01438 (15)
O2	0.8201 (5)	0.7193 (5)	0.6960 (5)	0.0181 (11)
O3	0.5530 (6)	0.8006 (6)	1.0157 (5)	0.0191 (11)
O1	0.7678 (6)	0.4158 (6)	0.9272 (5)	0.0221 (11)
C1	0.6804 (8)	0.4526 (8)	0.8620 (7)	0.0153 (14)
O7	0.1793 (6)	0.6493 (6)	0.8032 (5)	0.0186 (11)
H7	0.1438	0.5913	0.8449	0.028*
C4	0.1962 (8)	0.8155 (7)	0.8974 (7)	0.0141 (8)
H4C	0.2448	0.833	0.992	0.021*
H4A	0.0974	0.8365	0.9024	0.021*
H4B	0.2572	0.8837	0.8583	0.021*
O6	0.3692 (6)	0.5548 (6)	0.6216 (5)	0.0214 (11)
H6A	0.295 (9)	0.599 (9)	0.681 (8)	0.032*
H6B	0.406 (9)	0.640 (9)	0.575 (8)	0.032*

	U11	U22	U33	U12	U13	U23
Re01	0.00886 (14)	0.00633 (14)	0.00918 (13)	−0.00064 (10)	0.00140 (9)	0.00280 (10)
Br1	0.0139 (3)	0.0099 (3)	0.0110 (3)	0.0015 (3)	0.0039 (2)	0.0033 (2)
O4	0.016 (3)	0.006 (2)	0.010 (2)	0.001 (2)	0.0039 (18)	0.0042 (18)
C11	0.007 (3)	0.012 (3)	0.015 (3)	0.005 (3)	0.004 (2)	0.008 (3)
C2	0.024 (2)	0.0071 (19)	0.0122 (17)	0.0075 (18)	0.0005 (15)	0.0033 (15)
C15	0.010 (3)	0.017 (4)	0.014 (3)	0.002 (3)	−0.002 (2)	0.009 (3)
C3	0.024 (2)	0.0071 (19)	0.0122 (17)	0.0075 (18)	0.0005 (15)	0.0033 (15)
C17	0.010 (3)	0.007 (3)	0.010 (3)	0.001 (3)	0.000 (2)	0.006 (2)
O5	0.010 (2)	0.004 (2)	0.011 (2)	−0.0030 (19)	0.0036 (17)	−0.0002 (17)
C16	0.011 (3)	0.012 (3)	0.008 (3)	0.002 (3)	0.003 (2)	0.005 (3)
C12	0.006 (3)	0.013 (3)	0.007 (3)	0.001 (3)	0.001 (2)	0.005 (2)
C13	0.004 (3)	0.010 (3)	0.014 (3)	0.000 (3)	−0.002 (2)	0.004 (3)
C14	0.010 (3)	0.007 (3)	0.019 (3)	−0.004 (3)	−0.004 (3)	0.004 (3)
Br2	0.0181 (4)	0.0091 (3)	0.0225 (3)	−0.0015 (3)	0.0040 (3)	0.0052 (3)
Br3	0.0123 (3)	0.0144 (3)	0.0140 (3)	−0.0005 (3)	0.0057 (3)	0.0036 (3)
O2	0.016 (3)	0.015 (3)	0.025 (3)	0.001 (2)	0.010 (2)	0.011 (2)
O3	0.017 (3)	0.017 (3)	0.018 (2)	0.005 (2)	0.003 (2)	−0.001 (2)
O1	0.022 (3)	0.025 (3)	0.020 (3)	0.008 (2)	−0.001 (2)	0.010 (2)
C1	0.020 (4)	0.009 (3)	0.012 (3)	0.000 (3)	0.003 (3)	−0.001 (3)
O7	0.025 (3)	0.021 (3)	0.022 (3)	0.013 (2)	0.008 (2)	0.018 (2)
C4	0.024 (2)	0.0071 (19)	0.0122 (17)	0.0075 (18)	0.0005 (15)	0.0033 (15)
O6	0.025 (3)	0.025 (3)	0.025 (3)	0.013 (3)	0.008 (2)	0.018 (2)

Re01—C1	1.882 (7)	C3—O3	1.162 (8)
Re01—C3	1.897 (6)	C17—C16	1.415 (8)
Re01—C2	1.899 (7)	C16—Br3	1.895 (6)
Re01—O4	2.123 (5)	C12—C13	1.372 (9)
Re01—O5	2.146 (4)	C13—C14	1.378 (9)
Re01—O6	2.170 (5)	C13—H13	0.93
Br1—C12	1.899 (6)	C14—Br2	1.900 (6)
O4—C17	1.278 (7)	O1—C1	1.168 (8)
C11—O5	1.289 (7)	O7—C4	1.495 (8)
C11—C12	1.408 (9)	O7—H7	0.82
C11—C17	1.477 (8)	C4—H4C	0.96
C2—O2	1.171 (8)	C4—H4A	0.96
C15—C16	1.379 (9)	C4—H4B	0.96
C15—C14	1.398 (9)	O6—H6A	0.99 (8)
C15—H15	0.93	O6—H6B	1.06 (8)
C1—Re01—C3	89.5 (3)	C16—C17—C11	125.5 (6)
C1—Re01—C2	87.8 (3)	C11—O5—Re01	117.1 (4)
C3—Re01—C2	85.0 (3)	C15—C16—C17	131.3 (6)
C1—Re01—O4	96.2 (2)	C15—C16—Br3	113.9 (5)
C3—Re01—O4	99.6 (2)	C17—C16—Br3	114.6 (4)
C2—Re01—O4	173.9 (2)	C13—C12—C11	131.5 (6)
C1—Re01—O5	96.7 (2)	C13—C12—Br1	113.1 (4)
C3—Re01—O5	171.5 (2)	C11—C12—Br1	115.2 (5)
C2—Re01—O5	100.9 (2)	C12—C13—C14	128.9 (6)
O4—Re01—O5	74.07 (16)	C12—C13—H13	115.6
C1—Re01—O6	174.3 (3)	C14—C13—H13	115.6
C3—Re01—O6	94.2 (2)	C13—C14—C15	128.3 (6)
C2—Re01—O6	96.8 (2)	C13—C14—Br2	115.9 (5)
O4—Re01—O6	78.93 (19)	C15—C14—Br2	115.8 (5)
O5—Re01—O6	79.17 (18)	O1—C1—Re01	178.7 (6)
C17—O4—Re01	118.0 (4)	C4—O7—H7	109.5
O5—C11—C12	120.1 (5)	O7—C4—H4C	109.5
O5—C11—C17	115.0 (5)	O7—C4—H4A	109.5
C12—C11—C17	124.9 (6)	H4C—C4—H4A	109.5
O2—C2—Re01	177.7 (6)	O7—C4—H4B	109.5
C16—C15—C14	128.0 (6)	H4C—C4—H4B	109.5
C16—C15—H15	116	H4A—C4—H4B	109.5
C14—C15—H15	116	Re01—O6—H6A	110 (4)
O3—C3—Re01	179.1 (6)	Re01—O6—H6B	117 (4)
O4—C17—C16	119.0 (5)	H6A—O6—H6B	102 (6)
O4—C17—C11	115.4 (6)

D—H···A	D—H	H···A	D···A	D—H···A
O6—H6B···Br1i	1.06 (8)	2.68 (8)	3.421 (6)	127 (5)
O6—H6B···O5i	1.06 (8)	1.86 (8)	2.825 (7)	149 (6)
C15—H15···O2ii	0.93	2.5	3.409 (8)	166
O7—H7···O1iii	0.82	2.39	2.986 (7)	130
O6—H6A···O7	0.99 (8)	1.69 (8)	2.665 (7)	167 (7)

Re01—C1	1.882 (7)
Re01—C3	1.897 (6)
Re01—C2	1.899 (7)
Re01—O4	2.123 (5)
Re01—O5	2.146 (4)
Re01—O6	2.170 (5)

O4—Re01—O5	74.07 (16)
O4—Re01—O6	78.93 (19)
O5—Re01—O6	79.17 (18)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O6—H6B⋯Br1i	1.06 (8)	2.68 (8)	3.421 (6)	127 (5)
O6—H6B⋯O5i	1.06 (8)	1.86 (8)	2.825 (7)	149 (6)
C15—H15⋯O2ii	0.93	2.5	3.409 (8)	166
O7—H7⋯O1iii	0.82	2.39	2.986 (7)	130
O6—H6A⋯O7	0.99 (8)	1.69 (8)	2.665 (7)	167 (7)

Symmetry codes: (i) ; (ii) ; (iii) .