Bis(2-Amino-6-methyl­pyridinium) aqua­tetra­bromido­oxido­rhenate(V) bromide

Kochel, A.

doi:10.1107/S1600536807044133

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Bis(2-Amino-6-methylpyridinium) aquatetrabromidooxidorhenate(V) bromide

A. Kochel

The title compound, (C₆H₉N₂)₂·[ReO(H₂O)Br₄]·Br, is a molecular salt incorporating rhenium(V)-containing oxoanions. The oxoanion shows a distorted trans-ReO₂Br₄ geometry. In the crystal structure, the component species are connected via N—H

Br and O—H

Br interactions.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807044133/hb2535sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807044133/hb2535Isup2.hkl Contains datablock I

CCDC reference: 663596

checkCIF report

Key indicators

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.008 Å
R factor = 0.039
wR factor = 0.069
Data-to-parameter ratio = 42.3

checkCIF/PLATON results

No syntax errors found



Alert level C
CELLV02_ALERT_1_C  The supplied cell volume s.u. differs from that
            calculated from the cell parameter s.u.'s by > 2
            Calculated cell volume su =       9.11
            Cell volume su given      =       7.00
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent .....          ?
PLAT431_ALERT_2_C Short Inter HL..A Contact  Br2    ..  Br3     ..       3.57 Ang.
PLAT731_ALERT_1_C Bond    Calc     0.92(5), Rep   0.922(19) ......       2.63 su-Ra
              N2   -H2N     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.92(5), Rep   0.920(19) ......       2.63 su-Ra
              N3   -H4N     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.90(5), Rep   0.903(19) ......       2.63 su-Ra
              N4   -H5N     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.92(4), Rep   0.920(19) ......       2.11 su-Ra
              N4   -H6N     1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.95(4), Rep   0.948(19) ......       2.11 su-Ra
              O1   -H1W     1.555   1.555
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          3
              Br4 H2 O2 Re

Alert level G
ABSTM02_ALERT_3_G  The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
            Tmin and Tmax reported:      0.340     0.563
            Tmin(prime) and Tmax expected:      0.289     0.353
            RR(prime) =      0.738
            Please check that your absorption correction is appropriate.
PLAT794_ALERT_5_G Check Predicted Bond Valency for Re1         (3)       2.36
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          8

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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
   1 ALERT type 5 Informative message, check

Comment top

This paper reports the crystal structure of a molecular salt containing the [Re^VO(H₂O)Br₄]^- anion. All atoms lie on general positions (Fig. 1). The [ReO(H₂O)Br₄]^- anion in (I) shows a distorted trans-ReO₂Br₄ octahedral geometry about the central Re(V) ion (Table 1). The water molecule is weakly coordinated to rhenium at the base of octahedron with a Re—O distance of 2.206 (3) Å. The Re—Br bond lengths in (I) agree with those in related crystal structures (Abram et al., 1996; Chiozzone et al., 2006; Kochel, 2007).

In the crystal, the component species interact via N—H···Br and O—H···Br hydrogen bonds (Table 2), resulting in alternating layers of anions and cations perpendicular to [010] The shortest Re···Re distances in (I) are 6.819 (3) Å for Re1···Re1ⁱ (i = -x, -y + 2, -z + 1) and 8.546 (4) Å for Re1···Re2ⁱ (i = -x - 1, -y + 2, -z).

Related literature top

For related structures, see: Abram et al. (1996); Chiozzone et al. (2006); Kochel (2007). For synthetic background, see: Watt & Thompson (1963).

Experimental top

(NH₄)₂ReBr₆ was obtained by the method of Watt & Thompson (1963). A mixture of (NH₄)₂ReBr₆ (0.33 g) and 2-amino-6-methylpyridine (0.80 g) was dissolved in 50- ml of ethanol solution, which was heated at 323 K for 10 h followed by slow cooling. After the reaction the mixture colour was yellow–orange. The solution was filtered and the filtrate was left standing for evaporation. After five days, orange plates of (I) appeared. Anal. Calc for C₁₂H₂₀Br₅N₄O₂Re: C 17.19, H 2.57, N 6.68%; found C 16.34, H 2.30, N 6.54%. IR (KBr): 1195(versus), 1200(s), 990(m), 950(s), 1054(m), 980(s), 873(m), 810(s), 730(m), 310(s), 174(m), 159(m).

Structure description top

For related structures, see: Abram et al. (1996); Chiozzone et al. (2006); Kochel (2007). For synthetic background, see: Watt & Thompson (1963).

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis RED (Oxford Diffraction, 2003); data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); XP (Bruker, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).

Figures top

	Fig. 1. The molecular structure of (I) showing 50% displacement ellipsoids (arbitrary spheres for the H atoms).
	Fig. 2. The crystal packing in (I).

Bis(2-Amino-6-methylpyridinium) aquatetrabromidooxidorhenate(V) bromide top

Crystal data top

(C₆H₉N₂)₂·[ReO(H₂O)Br₄]·Br	F(000) = 1544
M_r = 838.07	D_x = 2.574 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 5614 reflections
a = 11.996 (2) Å	θ = 2.7–36.7°
b = 12.154 (3) Å	µ = 14.87 mm⁻¹
c = 18.206 (3) Å	T = 100 K
β = 125.43 (2)°	Prism, orange
V = 2162.9 (7) Å³	0.08 × 0.08 × 0.07 mm
Z = 4

Data collection top

Kuma KM4 CCD diffractometer	10288 independent reflections
Radiation source: fine-focus sealed tube	5873 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.080
ω scans	θ_max = 36.7°, θ_min = 2.7°
Absorption correction: numerical (CrysAlis [CrysAlis RED?]; Oxford Diffraction, 2003)	h = −19→19
T_min = 0.340, T_max = 0.563	k = −18→20
40507 measured reflections	l = −30→24

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.069	H atoms treated by a mixture of independent and constrained refinement
S = 0.92	w = 1/[σ²(F_o²) + (0.0236P)²] where P = (F_o² + 2F_c²)/3
10288 reflections	(Δ/σ)_max = 0.001
243 parameters	Δρ_max = 2.13 e Å⁻³
8 restraints	Δρ_min = −2.32 e Å⁻³

Crystal data top

(C₆H₉N₂)₂·[ReO(H₂O)Br₄]·Br	V = 2162.9 (7) Å³
M_r = 838.07	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.996 (2) Å	µ = 14.87 mm⁻¹
b = 12.154 (3) Å	T = 100 K
c = 18.206 (3) Å	0.08 × 0.08 × 0.07 mm
β = 125.43 (2)°

Data collection top

Kuma KM4 CCD diffractometer	10288 independent reflections
Absorption correction: numerical (CrysAlis [CrysAlis RED?]; Oxford Diffraction, 2003)	5873 reflections with I > 2σ(I)
T_min = 0.340, T_max = 0.563	R_int = 0.080
40507 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.039	8 restraints
wR(F²) = 0.069	H atoms treated by a mixture of independent and constrained refinement
S = 0.92	Δρ_max = 2.13 e Å⁻³
10288 reflections	Δρ_min = −2.32 e Å⁻³
243 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.

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	U_iso*/U_eq
N1	0.4220 (4)	0.6746 (3)	0.9044 (2)	0.0208 (7)
H1N	0.409 (5)	0.7471 (18)	0.911 (3)	0.025*
N2	0.1884 (4)	0.6673 (3)	0.8315 (3)	0.0324 (9)
H2N	0.104 (3)	0.634 (4)	0.797 (3)	0.039*
H3N	0.193 (5)	0.7408 (18)	0.844 (3)	0.039*
C2	0.3048 (4)	0.6156 (3)	0.8599 (3)	0.0229 (9)
C3	0.3142 (5)	0.5033 (3)	0.8462 (3)	0.0271 (10)
H3	0.2366	0.4591	0.8173	0.033*
C4	0.4377 (5)	0.4602 (4)	0.8757 (3)	0.0310 (11)
H4	0.4440	0.3861	0.8658	0.037*
C5	0.5566 (5)	0.5257 (4)	0.9212 (3)	0.0318 (11)
H5	0.6406	0.4953	0.9406	0.038*
C6	0.5479 (4)	0.6329 (4)	0.9365 (3)	0.0261 (9)
C7	0.6656 (5)	0.7116 (5)	0.9858 (4)	0.0397 (13)
H7A	0.6761	0.7364	1.0396	0.060*
H7B	0.6482	0.7736	0.9478	0.060*
H7C	0.7478	0.6753	1.0016	0.060*
N3	0.1990 (3)	0.6251 (3)	0.5887 (2)	0.0182 (7)
H4N	0.265 (3)	0.621 (4)	0.578 (3)	0.022*
N4	0.2592 (4)	0.4446 (3)	0.6379 (3)	0.0278 (8)
H5N	0.334 (3)	0.457 (4)	0.639 (3)	0.033*
H6N	0.239 (5)	0.379 (2)	0.653 (3)	0.033*
C11	0.1736 (4)	0.5308 (3)	0.6153 (3)	0.0205 (8)
C12	0.0562 (5)	0.5275 (4)	0.6155 (3)	0.0275 (10)
H12	0.0324	0.4632	0.6311	0.033*
C13	−0.0216 (5)	0.6198 (4)	0.5926 (3)	0.0321 (11)
H13	−0.0980	0.6187	0.5938	0.039*
C14	0.0113 (5)	0.7163 (4)	0.5672 (3)	0.0288 (10)
H14	−0.0421	0.7791	0.5527	0.035*
C15	0.1211 (4)	0.7179 (3)	0.5638 (3)	0.0212 (8)
C16	0.1635 (4)	0.8130 (3)	0.5331 (3)	0.0250 (9)
H16A	0.1512	0.7943	0.4776	0.038*
H16B	0.2581	0.8296	0.5781	0.038*
H16C	0.1086	0.8760	0.5239	0.038*
Re1	−0.237586 (16)	0.926025 (12)	0.281334 (11)	0.01677 (4)
Br1	−0.06351 (4)	1.03636 (3)	0.27687 (3)	0.02292 (9)
Br2	−0.38484 (4)	1.09524 (3)	0.23272 (3)	0.02134 (9)
Br3	−0.44110 (4)	0.81224 (3)	0.23999 (3)	0.02152 (9)
Br4	−0.12108 (4)	0.75203 (3)	0.28299 (3)	0.02382 (9)
O1	−0.3328 (3)	0.9120 (2)	0.1355 (2)	0.0197 (6)
O2	−0.1646 (3)	0.9336 (2)	0.3918 (2)	0.0248 (6)
Br5	0.34325 (4)	0.88956 (3)	0.98187 (3)	0.02261 (9)
H1W	−0.324 (5)	0.978 (2)	0.111 (3)	0.027*
H2W	−0.426 (2)	0.897 (4)	0.088 (2)	0.027*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
N1	0.0184 (17)	0.0190 (16)	0.027 (2)	−0.0032 (14)	0.0139 (16)	−0.0034 (14)
N2	0.0181 (19)	0.029 (2)	0.041 (3)	−0.0060 (17)	0.0119 (19)	−0.0156 (18)
C2	0.024 (2)	0.025 (2)	0.020 (2)	−0.0060 (18)	0.0128 (19)	−0.0040 (17)
C3	0.035 (3)	0.023 (2)	0.029 (3)	−0.0080 (19)	0.021 (2)	−0.0075 (18)
C4	0.045 (3)	0.022 (2)	0.026 (2)	0.008 (2)	0.021 (2)	−0.0002 (18)
C5	0.026 (2)	0.039 (3)	0.029 (3)	0.014 (2)	0.015 (2)	−0.001 (2)
C6	0.021 (2)	0.037 (2)	0.024 (2)	−0.0022 (19)	0.015 (2)	−0.0027 (19)
C7	0.021 (2)	0.054 (3)	0.047 (3)	−0.012 (2)	0.021 (2)	−0.015 (3)
N3	0.0143 (16)	0.0228 (17)	0.0180 (17)	0.0015 (14)	0.0096 (15)	−0.0032 (13)
N4	0.031 (2)	0.0208 (19)	0.035 (2)	0.0061 (17)	0.0214 (19)	0.0049 (16)
C11	0.024 (2)	0.0206 (19)	0.014 (2)	−0.0007 (17)	0.0095 (18)	0.0008 (15)
C12	0.024 (2)	0.034 (2)	0.028 (3)	−0.0007 (19)	0.017 (2)	0.0030 (19)
C13	0.022 (2)	0.045 (3)	0.037 (3)	0.004 (2)	0.021 (2)	0.006 (2)
C14	0.021 (2)	0.029 (2)	0.034 (3)	0.0073 (19)	0.015 (2)	0.004 (2)
C15	0.022 (2)	0.0206 (19)	0.018 (2)	0.0020 (17)	0.0097 (18)	0.0008 (16)
C16	0.022 (2)	0.0187 (19)	0.027 (2)	0.0003 (17)	0.010 (2)	0.0014 (17)
Re1	0.01591 (7)	0.01429 (7)	0.01882 (8)	0.00079 (6)	0.00933 (6)	0.00002 (6)
Br1	0.0185 (2)	0.01779 (18)	0.0319 (2)	−0.00143 (16)	0.01433 (19)	−0.00067 (16)
Br2	0.0206 (2)	0.01803 (18)	0.0250 (2)	0.00517 (15)	0.01295 (18)	0.00171 (15)
Br3	0.0198 (2)	0.02158 (19)	0.0243 (2)	−0.00228 (16)	0.01344 (18)	0.00220 (16)
Br4	0.0198 (2)	0.01426 (18)	0.0349 (3)	0.00186 (15)	0.01442 (19)	−0.00040 (16)
O1	0.0256 (15)	0.0159 (13)	0.0201 (15)	0.0004 (12)	0.0147 (13)	0.0013 (11)
O2	0.0258 (15)	0.0221 (14)	0.0218 (16)	0.0022 (13)	0.0111 (13)	0.0022 (12)
Br5	0.0247 (2)	0.02478 (19)	0.0205 (2)	−0.00570 (17)	0.01438 (18)	−0.00151 (16)

Geometric parameters (Å, º) top

N1—C2	1.352 (5)	N4—H5N	0.903 (19)
N1—C6	1.363 (5)	N4—H6N	0.920 (19)
N1—H1N	0.913 (19)	C11—C12	1.411 (6)
N2—C2	1.331 (6)	C12—C13	1.361 (6)
N2—H2N	0.922 (19)	C12—H12	0.9300
N2—H3N	0.915 (19)	C13—C14	1.399 (6)
C2—C3	1.404 (6)	C13—H13	0.9300
C3—C4	1.354 (6)	C14—C15	1.354 (6)
C3—H3	0.9300	C14—H14	0.9300
C4—C5	1.410 (7)	C15—C16	1.496 (6)
C4—H4	0.9300	C16—H16A	0.9600
C5—C6	1.349 (6)	C16—H16B	0.9600
C5—H5	0.9300	C16—H16C	0.9600
C6—C7	1.498 (6)	Re1—O2	1.667 (3)
C7—H7A	0.9600	Re1—O1	2.206 (3)
C7—H7B	0.9600	Re1—Br3	2.5117 (6)
C7—H7C	0.9600	Re1—Br2	2.5141 (6)
N3—C11	1.347 (5)	Re1—Br1	2.5223 (5)
N3—C15	1.363 (5)	Re1—Br4	2.5254 (6)
N3—H4N	0.920 (19)	O1—H1W	0.948 (19)
N4—C11	1.354 (5)	O1—H2W	0.955 (19)

C2—N1—C6	124.7 (4)	C13—C12—C11	118.9 (4)
C2—N1—H1N	113 (3)	C13—C12—H12	120.6
C6—N1—H1N	122 (3)	C11—C12—H12	120.6
C2—N2—H2N	124 (3)	C12—C13—C14	121.2 (4)
C2—N2—H3N	118 (3)	C12—C13—H13	119.4
H2N—N2—H3N	118 (4)	C14—C13—H13	119.4
N2—C2—N1	118.4 (4)	C15—C14—C13	119.7 (4)
N2—C2—C3	124.3 (4)	C15—C14—H14	120.2
N1—C2—C3	117.3 (4)	C13—C14—H14	120.2
C4—C3—C2	119.2 (4)	C14—C15—N3	118.1 (4)
C4—C3—H3	120.4	C14—C15—C16	125.4 (4)
C2—C3—H3	120.4	N3—C15—C16	116.5 (4)
C3—C4—C5	121.1 (4)	C15—C16—H16A	109.5
C3—C4—H4	119.5	C15—C16—H16B	109.5
C5—C4—H4	119.5	H16A—C16—H16B	109.5
C6—C5—C4	119.6 (4)	C15—C16—H16C	109.5
C6—C5—H5	120.2	H16A—C16—H16C	109.5
C4—C5—H5	120.2	H16B—C16—H16C	109.5
C5—C6—N1	118.1 (4)	O2—Re1—O1	178.68 (12)
C5—C6—C7	125.6 (4)	O2—Re1—Br3	97.54 (10)
N1—C6—C7	116.4 (4)	O1—Re1—Br3	82.06 (8)
C6—C7—H7A	109.5	O2—Re1—Br2	98.64 (10)
C6—C7—H7B	109.5	O1—Re1—Br2	82.62 (7)
H7A—C7—H7B	109.5	Br3—Re1—Br2	88.99 (2)
C6—C7—H7C	109.5	O2—Re1—Br1	98.28 (10)
H7A—C7—H7C	109.5	O1—Re1—Br1	82.12 (8)
H7B—C7—H7C	109.5	Br3—Re1—Br1	164.174 (16)
C11—N3—C15	124.7 (3)	Br2—Re1—Br1	88.83 (2)
C11—N3—H4N	116 (3)	O2—Re1—Br4	97.56 (10)
C15—N3—H4N	119 (3)	O1—Re1—Br4	81.18 (7)
C11—N4—H5N	116 (3)	Br3—Re1—Br4	88.71 (2)
C11—N4—H6N	118 (3)	Br2—Re1—Br4	163.793 (16)
H5N—N4—H6N	125 (4)	Br1—Re1—Br4	89.02 (2)
N3—C11—N4	118.5 (4)	Re1—O1—H1W	112 (3)
N3—C11—C12	117.4 (4)	Re1—O1—H2W	129 (3)
N4—C11—C12	124.1 (4)	H1W—O1—H2W	97 (4)

C6—N1—C2—N2	−179.4 (4)	C15—N3—C11—N4	179.7 (4)
C6—N1—C2—C3	0.2 (6)	C15—N3—C11—C12	1.5 (6)
N2—C2—C3—C4	178.0 (4)	N3—C11—C12—C13	−2.6 (6)
N1—C2—C3—C4	−1.6 (6)	N4—C11—C12—C13	179.2 (4)
C2—C3—C4—C5	1.2 (7)	C11—C12—C13—C14	1.4 (7)
C3—C4—C5—C6	0.6 (7)	C12—C13—C14—C15	1.1 (7)
C4—C5—C6—N1	−2.0 (7)	C13—C14—C15—N3	−2.2 (7)
C4—C5—C6—C7	178.3 (5)	C13—C14—C15—C16	176.5 (4)
C2—N1—C6—C5	1.6 (6)	C11—N3—C15—C14	1.0 (6)
C2—N1—C6—C7	−178.7 (4)	C11—N3—C15—C16	−177.8 (4)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N···Br5	0.92 (3)	2.54 (5)	3.354 (4)	148 (5)
O1—H1W···Br5ⁱ	0.95 (4)	2.25 (4)	3.176 (3)	165 (4)
N2—H2N···Br1ⁱⁱ	0.92 (5)	2.76 (5)	3.573 (5)	148 (4)
N2—H2N···Br4ⁱⁱ	0.92 (5)	2.91 (5)	3.424 (6)	117 (4)
O1—H2W···Br5ⁱⁱⁱ	0.95 (3)	2.28 (3)	3.225 (4)	170 (4)
N2—H3N···Br5	0.92 (2)	2.75 (4)	3.514 (4)	141 (3)
N3—H4N···Br5^iv	0.92 (5)	2.42 (5)	3.273 (4)	154 (4)
N4—H5N···Br2^v	0.90 (5)	2.83 (5)	3.592 (6)	143 (4)
N4—H6N···Br4^vi	0.92 (4)	2.79 (5)	3.647 (5)	155 (5)

Symmetry codes: (i) −x, −y+2, −z+1; (ii) x, −y+3/2, z+1/2; (iii) x−1, y, z−1; (iv) x, −y+3/2, z−1/2; (v) x+1, −y+3/2, z+1/2; (vi) −x, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	(C₆H₉N₂)₂·[ReO(H₂O)Br₄]·Br
M_r	838.07
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	100
a, b, c (Å)	11.996 (2), 12.154 (3), 18.206 (3)
β (°)	125.43 (2)
V (Å³)	2162.9 (7)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	14.87
Crystal size (mm)	0.08 × 0.08 × 0.07

Data collection
Diffractometer	Kuma KM4 CCD
Absorption correction	Numerical (CrysAlis [CrysAlis RED?]; Oxford Diffraction, 2003)
T_min, T_max	0.340, 0.563
No. of measured, independent and observed [I > 2σ(I)] reflections	40507, 10288, 5873
R_int	0.080
(sin θ/λ)_max (Å⁻¹)	0.840

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.069, 0.92
No. of reflections	10288
No. of parameters	243
No. of restraints	8
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	2.13, −2.32

Computer programs: CrysAlis CCD (Oxford Diffraction, 2003), CrysAlis RED (Oxford Diffraction, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 2003); XP (Bruker, 1999).

Selected bond lengths (Å) top

Re1—O2	1.667 (3)	Re1—Br2	2.5141 (6)
Re1—O1	2.206 (3)	Re1—Br1	2.5223 (5)
Re1—Br3	2.5117 (6)	Re1—Br4	2.5254 (6)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N···Br5	0.92 (3)	2.54 (5)	3.354 (4)	148 (5)
O1—H1W···Br5ⁱ	0.95 (4)	2.25 (4)	3.176 (3)	165 (4)
N2—H2N···Br1ⁱⁱ	0.92 (5)	2.76 (5)	3.573 (5)	148 (4)
N2—H2N···Br4ⁱⁱ	0.92 (5)	2.91 (5)	3.424 (6)	117 (4)
O1—H2W···Br5ⁱⁱⁱ	0.95 (3)	2.28 (3)	3.225 (4)	170 (4)
N2—H3N···Br5	0.92 (2)	2.75 (4)	3.514 (4)	141 (3)
N3—H4N···Br5^iv	0.92 (5)	2.42 (5)	3.273 (4)	154 (4)
N4—H5N···Br2^v	0.90 (5)	2.83 (5)	3.592 (6)	143 (4)
N4—H6N···Br4^vi	0.92 (4)	2.79 (5)	3.647 (5)	155 (5)

Symmetry codes: (i) −x, −y+2, −z+1; (ii) x, −y+3/2, z+1/2; (iii) x−1, y, z−1; (iv) x, −y+3/2, z−1/2; (v) x+1, −y+3/2, z+1/2; (vi) −x, −y+1, −z+1.

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