Tetra-μ(3)-hydroxido-tetra-kis-[tricarbonyl-rhenium(I)] pyridine tetra-solvate.

The title compound, [Re(4)(μ(3)-OH)(4)(CO)(12)]·4C(5)H(5)N, crystallizes with one tetranuclear rhenium(I) cubane-like molecule and four pyridine mol-ecules in the asymmetric unit. The coordination environment of each Re(I) atom is distorted octahedral. Four intra-molecular O-H⋯N and four inter-molecular C-H⋯O hydrogen-bond inter-actions are observed. Relatively strong hydrogen bonds are found between the hydrogen-bond donor (μ(3)-OH) and acceptor (basic N atom of pyridine), with N⋯O distances between 2.586 (10) and 2.628 (10) Å. Inter-cube distances of 9.873 (2) and 12.376 (3) Å are observed.

Related literature

For similar structures, see: Herberhold & Süss (1975 ▶); Nuber et al. (1981 ▶); Copp et al. (1995 ▶); Egli et al. (1997 ▶). For the synthesis of the precursor, see: Alberto et al. (1996 ▶).

Experimental

Crystal data

[Re4(OH)4(CO)12]·4C5H5N

M = 1465.39

Monoclinic,

a = 11.895 (5) Å

b = 21.847 (5) Å

c = 16.245 (5) Å

β = 109.707 (5)°

V = 3974 (2) Å3

Z = 4

Mo Kα radiation

μ = 12.22 mm−1

T = 100 K

0.43 × 0.11 × 0.11 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2008 ▶) T min = 0.211, T max = 0.271

68439 measured reflections

9594 independent reflections

7966 reflections with I > 2σ(I)

R int = 0.064

Refinement

R[F 2 > 2σ(F 2)] = 0.043

wR(F 2) = 0.099

S = 1.04

9594 reflections

516 parameters

4 restraints

H atoms treated by a mixture of independent and constrained refinement

Δρmax = 7.00 e Å−3

Δρmin = −6.09 e Å−3

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT-Plus (Bruker, 2008 ▶); 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 (Brandenburg & Putz, 2005 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812036033/hg5243sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812036033/hg5243Isup2.hkl

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

[Re4(OH)4(CO)12]·4C5H5N	F(000) = 2688
Mr = 1465.39	Dx = 2.449 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9793 reflections
a = 11.895 (5) Å	θ = 2.7–28.1°
b = 21.847 (5) Å	µ = 12.22 mm−1
c = 16.245 (5) Å	T = 100 K
β = 109.707 (5)°	Cuboid, colourless
V = 3974 (2) Å3	0.43 × 0.11 × 0.11 mm
Z = 4

Bruker APEXII CCD diffractometer	7966 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.064
φ and ω scans	θmax = 28°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Bruker, 2008)	h = −15→15
Tmin = 0.211, Tmax = 0.271	k = −28→28
68439 measured reflections	l = −20→21
9594 independent reflections

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)] = 0.043	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ2(Fo2) + (0.0181P)2 + 118.6736P] where P = (Fo2 + 2Fc2)/3
9594 reflections	(Δ/σ)max = 0.001
516 parameters	Δρmax = 7.00 e Å−3
4 restraints	Δρmin = −6.09 e Å−3

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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 > 2σ(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
Re3	0.36392 (3)	0.330517 (15)	0.69816 (2)	0.01378 (7)
Re4	0.36579 (3)	0.431796 (15)	0.85997 (2)	0.01378 (7)
Re2	0.16248 (3)	0.316708 (15)	0.80536 (2)	0.01277 (8)
O1	0.1755 (6)	0.3368 (3)	0.6780 (4)	0.0146 (12)
O33	0.6355 (6)	0.3461 (4)	0.7514 (4)	0.0299 (17)
C23	−0.0056 (8)	0.3095 (4)	0.7695 (5)	0.0146 (17)
O4	0.3333 (6)	0.4265 (3)	0.7203 (4)	0.0154 (12)
O23	−0.1098 (6)	0.3044 (3)	0.7458 (4)	0.0235 (14)
Re1	0.14174 (3)	0.434793 (15)	0.66166 (2)	0.01489 (8)
O3	0.3485 (5)	0.3351 (3)	0.8273 (4)	0.0128 (12)
O41	0.3519 (6)	0.5714 (3)	0.8711 (5)	0.0258 (15)
O42	0.3772 (6)	0.4234 (3)	1.0504 (4)	0.0217 (14)
O43	0.6378 (6)	0.4340 (3)	0.9300 (4)	0.0257 (15)
C43	0.5348 (8)	0.4345 (4)	0.9030 (5)	0.0147 (17)
C42	0.3727 (8)	0.4268 (4)	0.9792 (6)	0.0195 (19)
C41	0.3593 (8)	0.5192 (4)	0.8685 (6)	0.0178 (18)
O31	0.3407 (7)	0.3349 (3)	0.5051 (4)	0.0277 (16)
O21	0.1723 (7)	0.3090 (4)	0.9962 (4)	0.0331 (18)
C31	0.3503 (8)	0.3337 (4)	0.5783 (6)	0.0189 (18)
C21	0.1686 (9)	0.3116 (4)	0.9247 (6)	0.022 (2)
C33	0.5327 (9)	0.3392 (5)	0.7306 (5)	0.021 (2)
O22	0.1678 (7)	0.1772 (3)	0.7977 (5)	0.0332 (17)
C22	0.1671 (8)	0.2291 (4)	0.8013 (6)	0.0192 (18)
O32	0.3974 (7)	0.1929 (3)	0.6811 (4)	0.0304 (17)
O11	0.1210 (8)	0.5739 (3)	0.6689 (6)	0.045 (2)
C32	0.3824 (9)	0.2454 (5)	0.6885 (6)	0.021 (2)
C11	0.1278 (9)	0.5215 (5)	0.6665 (7)	0.027 (2)
O12	0.1361 (7)	0.4482 (4)	0.4735 (5)	0.0336 (18)
C12	0.1361 (9)	0.4431 (4)	0.5446 (6)	0.023 (2)
C13	−0.0265 (9)	0.4291 (4)	0.6207 (6)	0.0206 (19)
O13	−0.1292 (7)	0.4231 (3)	0.5947 (5)	0.0320 (17)
N1	0.5054 (7)	0.2663 (4)	0.9429 (5)	0.0211 (17)
N2	0.0085 (8)	0.2811 (4)	0.5546 (5)	0.0247 (18)
N3	0.0328 (7)	0.4768 (4)	0.8558 (5)	0.0226 (17)
N4	0.4824 (7)	0.4935 (4)	0.6715 (5)	0.0224 (17)
C305	−0.0787 (10)	0.4596 (5)	0.8305 (7)	0.032 (2)
H305	−0.0992	0.4236	0.7984	0.038*
C302	−0.0225 (13)	0.5632 (6)	0.9231 (9)	0.047 (3)
H302	0.0003	0.5985	0.9566	0.056*
C304	−0.1692 (11)	0.4915 (6)	0.8484 (8)	0.040 (3)
H304	−0.2472	0.4769	0.83	0.047*
C303	−0.1390 (11)	0.5454 (6)	0.8941 (9)	0.042 (3)
H303	−0.1971	0.5693	0.905	0.05*
C301	0.0622 (11)	0.5286 (5)	0.9025 (8)	0.035 (3)
H301	0.1412	0.5417	0.9216	0.042*
C403	0.6711 (9)	0.5524 (5)	0.6397 (7)	0.026 (2)
H403	0.7338	0.572	0.6285	0.031*
C402	0.6276 (9)	0.4985 (5)	0.5998 (6)	0.024 (2)
H402	0.6607	0.4807	0.5613	0.029*
C401	0.5332 (9)	0.4701 (5)	0.6170 (6)	0.027 (2)
H401	0.5043	0.4332	0.5893	0.032*
C404	0.6207 (10)	0.5777 (5)	0.6972 (7)	0.029 (2)
H404	0.6495	0.6142	0.7261	0.035*
C405	0.5257 (10)	0.5471 (5)	0.7108 (7)	0.028 (2)
H405	0.4905	0.5644	0.7485	0.034*
C205	−0.0490 (10)	0.2326 (5)	0.5699 (7)	0.033 (2)
H205	−0.0253	0.2164	0.6261	0.039*
C201	−0.0277 (11)	0.3038 (5)	0.4733 (7)	0.035 (3)
H201	0.0107	0.3382	0.462	0.042*
C204	−0.1424 (11)	0.2052 (6)	0.5054 (9)	0.048 (4)
H204	−0.181	0.1715	0.5184	0.058*
C203	−0.1781 (12)	0.2284 (7)	0.4218 (9)	0.052 (4)
H203	−0.2405	0.2105	0.3772	0.062*
C202	−0.1194 (13)	0.2784 (7)	0.4058 (8)	0.053 (4)
H202	−0.1412	0.295	0.35	0.063*
C105	0.5525 (9)	0.2822 (5)	1.0269 (6)	0.023 (2)
H105	0.5308	0.3196	1.0443	0.027*
C103	0.6650 (9)	0.1902 (5)	1.0643 (6)	0.024 (2)
H103	0.7184	0.1646	1.1048	0.029*
C104	0.6325 (9)	0.2455 (5)	1.0898 (6)	0.027 (2)
H104	0.6633	0.2581	1.1477	0.032*
C102	0.6167 (10)	0.1732 (5)	0.9773 (6)	0.028 (2)
H102	0.6372	0.136	0.9583	0.034*
C101	0.5376 (10)	0.2124 (5)	0.9189 (6)	0.027 (2)
H101	0.5055	0.2007	0.8606	0.032*
O2	0.1773 (6)	0.4152 (3)	0.7990 (4)	0.0166 (13)
H3	0.395 (10)	0.316 (6)	0.871 (6)	0.06 (4)*
H2	0.134 (8)	0.436 (4)	0.821 (6)	0.02 (3)*
H1	0.127 (11)	0.319 (6)	0.634 (6)	0.07 (5)*
H4	0.376 (11)	0.452 (5)	0.704 (9)	0.07 (5)*

	U11	U22	U33	U12	U13	U23
Re3	0.01351 (13)	0.01541 (12)	0.01219 (11)	0.00124 (9)	0.00403 (9)	0.00039 (8)
Re4	0.01351 (13)	0.01541 (12)	0.01219 (11)	0.00124 (9)	0.00403 (9)	0.00039 (8)
Re2	0.01148 (17)	0.01394 (16)	0.01229 (15)	−0.00146 (12)	0.00322 (12)	−0.00020 (12)
O1	0.014 (3)	0.014 (3)	0.010 (3)	0.002 (2)	−0.003 (2)	0.000 (2)
O33	0.013 (4)	0.053 (5)	0.023 (3)	0.006 (3)	0.004 (3)	0.005 (3)
C23	0.017 (5)	0.015 (4)	0.010 (4)	−0.005 (3)	0.003 (3)	0.000 (3)
O4	0.019 (3)	0.014 (3)	0.016 (3)	0.001 (3)	0.009 (3)	0.005 (2)
O23	0.016 (4)	0.022 (3)	0.032 (4)	−0.002 (3)	0.008 (3)	0.004 (3)
Re1	0.01131 (17)	0.01397 (16)	0.01761 (16)	0.00153 (13)	0.00254 (13)	0.00234 (12)
O3	0.013 (3)	0.013 (3)	0.011 (3)	−0.001 (2)	0.003 (2)	0.000 (2)
O41	0.028 (4)	0.012 (3)	0.034 (4)	−0.006 (3)	0.006 (3)	−0.004 (3)
O42	0.021 (4)	0.029 (4)	0.017 (3)	−0.006 (3)	0.009 (3)	−0.003 (3)
O43	0.017 (4)	0.030 (4)	0.030 (4)	−0.007 (3)	0.008 (3)	−0.001 (3)
C43	0.015 (4)	0.014 (4)	0.016 (4)	−0.004 (3)	0.007 (3)	−0.004 (3)
C42	0.015 (5)	0.013 (4)	0.029 (5)	−0.003 (3)	0.006 (4)	−0.001 (4)
C41	0.015 (4)	0.016 (4)	0.020 (4)	−0.001 (3)	0.003 (4)	0.002 (3)
O31	0.034 (4)	0.034 (4)	0.016 (3)	0.005 (3)	0.009 (3)	0.002 (3)
O21	0.038 (5)	0.049 (5)	0.016 (3)	−0.012 (4)	0.014 (3)	−0.002 (3)
C31	0.019 (5)	0.022 (4)	0.015 (4)	0.004 (4)	0.003 (3)	0.001 (3)
C21	0.016 (5)	0.019 (4)	0.027 (5)	−0.005 (4)	0.002 (4)	−0.002 (4)
C33	0.023 (5)	0.031 (5)	0.006 (4)	0.008 (4)	0.002 (3)	−0.001 (3)
O22	0.035 (4)	0.018 (4)	0.040 (4)	0.001 (3)	0.005 (3)	0.000 (3)
C22	0.012 (4)	0.018 (4)	0.023 (4)	0.000 (3)	0.001 (4)	0.000 (4)
O32	0.050 (5)	0.017 (3)	0.024 (3)	0.008 (3)	0.012 (3)	0.000 (3)
O11	0.047 (5)	0.013 (4)	0.056 (5)	0.003 (3)	−0.007 (4)	0.003 (3)
C32	0.019 (5)	0.029 (5)	0.014 (4)	−0.004 (4)	0.003 (4)	0.002 (4)
C11	0.016 (5)	0.025 (5)	0.027 (5)	0.003 (4)	−0.008 (4)	0.005 (4)
O12	0.033 (4)	0.039 (4)	0.026 (4)	0.006 (3)	0.006 (3)	0.016 (3)
C12	0.016 (5)	0.023 (5)	0.023 (5)	0.004 (4)	−0.001 (4)	0.010 (4)
C13	0.015 (5)	0.020 (4)	0.021 (4)	0.004 (4)	−0.001 (4)	0.000 (4)
O13	0.022 (4)	0.029 (4)	0.042 (4)	0.002 (3)	0.006 (3)	0.005 (3)
N1	0.020 (4)	0.027 (4)	0.015 (3)	−0.004 (3)	0.004 (3)	0.003 (3)
N2	0.022 (4)	0.022 (4)	0.026 (4)	0.000 (3)	0.003 (3)	−0.007 (3)
N3	0.018 (4)	0.022 (4)	0.029 (4)	0.003 (3)	0.009 (3)	−0.005 (3)
N4	0.022 (4)	0.024 (4)	0.023 (4)	−0.003 (3)	0.009 (3)	0.003 (3)
C305	0.029 (6)	0.032 (6)	0.038 (6)	0.001 (5)	0.016 (5)	0.004 (5)
C302	0.067 (10)	0.029 (6)	0.052 (7)	0.015 (6)	0.030 (7)	−0.011 (5)
C304	0.025 (6)	0.047 (7)	0.052 (7)	0.006 (5)	0.020 (5)	0.014 (6)
C303	0.037 (7)	0.041 (7)	0.057 (8)	0.015 (6)	0.029 (6)	0.000 (6)
C301	0.031 (6)	0.030 (6)	0.047 (7)	0.002 (5)	0.016 (5)	−0.007 (5)
C403	0.026 (5)	0.025 (5)	0.031 (5)	0.000 (4)	0.016 (4)	0.011 (4)
C402	0.019 (5)	0.034 (5)	0.022 (5)	−0.001 (4)	0.010 (4)	0.002 (4)
C401	0.026 (6)	0.031 (5)	0.022 (5)	−0.008 (4)	0.006 (4)	−0.006 (4)
C404	0.031 (6)	0.017 (5)	0.042 (6)	−0.005 (4)	0.015 (5)	−0.005 (4)
C405	0.034 (6)	0.025 (5)	0.034 (5)	0.007 (4)	0.021 (5)	0.002 (4)
C205	0.030 (6)	0.035 (6)	0.034 (6)	0.002 (5)	0.011 (5)	−0.015 (5)
C201	0.041 (7)	0.031 (6)	0.023 (5)	0.013 (5)	−0.001 (5)	−0.005 (4)
C204	0.033 (7)	0.045 (7)	0.069 (9)	−0.017 (6)	0.020 (7)	−0.035 (7)
C203	0.030 (7)	0.062 (9)	0.046 (7)	0.010 (6)	−0.009 (6)	−0.039 (7)
C202	0.054 (9)	0.067 (9)	0.024 (6)	0.016 (7)	−0.005 (6)	−0.024 (6)
C105	0.025 (5)	0.023 (5)	0.020 (4)	0.003 (4)	0.007 (4)	0.001 (4)
C103	0.025 (5)	0.024 (5)	0.022 (5)	0.004 (4)	0.006 (4)	0.005 (4)
C104	0.026 (6)	0.033 (5)	0.015 (4)	−0.001 (4)	−0.002 (4)	0.003 (4)
C102	0.035 (6)	0.029 (5)	0.022 (5)	0.015 (5)	0.010 (4)	0.003 (4)
C101	0.032 (6)	0.026 (5)	0.020 (5)	0.001 (4)	0.005 (4)	0.003 (4)
O2	0.021 (3)	0.015 (3)	0.017 (3)	0.001 (3)	0.010 (3)	−0.002 (2)

Re3—C32	1.886 (10)	N2—C201	1.339 (13)
Re3—C31	1.900 (9)	N3—C305	1.304 (14)
Re3—C33	1.906 (10)	N3—C301	1.342 (13)
Re3—O1	2.157 (6)	N4—C401	1.331 (13)
Re3—O3	2.168 (6)	N4—C405	1.349 (13)
Re3—O4	2.179 (6)	C305—C304	1.392 (16)
Re4—C43	1.893 (9)	C305—H305	0.93
Re4—C42	1.913 (10)	C302—C303	1.362 (19)
Re4—C41	1.918 (9)	C302—C301	1.386 (16)
Re4—O2	2.154 (7)	C302—H302	0.93
Re4—O3	2.172 (6)	C304—C303	1.373 (18)
Re4—O4	2.173 (6)	C304—H304	0.93
Re2—C23	1.891 (9)	C303—H303	0.93
Re2—C22	1.916 (9)	C301—H301	0.93
Re2—C21	1.918 (10)	C403—C402	1.359 (14)
Re2—O3	2.157 (6)	C403—C404	1.385 (14)
Re2—O2	2.165 (6)	C403—H403	0.93
Re2—O1	2.171 (6)	C402—C401	1.392 (14)
O1—Re1	2.178 (6)	C402—H402	0.93
O1—H1	0.85 (2)	C401—H401	0.93
O33—C33	1.164 (12)	C404—C405	1.392 (15)
C23—O23	1.173 (11)	C404—H404	0.93
O4—Re1	2.160 (6)	C405—H405	0.93
O4—H4	0.85 (2)	C205—C204	1.380 (16)
Re1—C12	1.888 (10)	C205—H205	0.93
Re1—C13	1.889 (10)	C201—C202	1.376 (16)
Re1—C11	1.907 (10)	C201—H201	0.93
Re1—O2	2.169 (6)	C204—C203	1.38 (2)
O3—H3	0.85 (2)	C204—H204	0.93
O41—C41	1.146 (11)	C203—C202	1.37 (2)
O42—C42	1.143 (11)	C203—H203	0.93
O43—C43	1.154 (11)	C202—H202	0.93
O31—C31	1.156 (11)	C105—C104	1.391 (13)
O21—C21	1.149 (11)	C105—H105	0.93
O22—C22	1.137 (11)	C103—C104	1.375 (14)
O32—C32	1.172 (12)	C103—C102	1.386 (13)
O11—C11	1.149 (12)	C103—H103	0.93
O12—C12	1.161 (12)	C104—H104	0.93
C13—O13	1.157 (12)	C102—C101	1.384 (14)
N1—C105	1.334 (12)	C102—H102	0.93
N1—C101	1.338 (13)	C101—H101	0.93
N2—C205	1.328 (14)	O2—H2	0.85 (2)
C32—Re3—C31	85.6 (4)	O42—C42—Re4	179.5 (9)
C32—Re3—C33	88.8 (4)	O41—C41—Re4	177.6 (8)
C31—Re3—C33	89.8 (4)	O31—C31—Re3	178.9 (9)
C32—Re3—O1	101.2 (3)	O21—C21—Re2	179.5 (9)
C31—Re3—O1	96.7 (3)	O33—C33—Re3	178.0 (9)
C33—Re3—O1	168.4 (3)	O22—C22—Re2	178.7 (9)
C32—Re3—O3	100.1 (3)	O32—C32—Re3	177.3 (9)
C31—Re3—O3	169.7 (3)	O11—C11—Re1	178.9 (11)
C33—Re3—O3	98.8 (3)	O12—C12—Re1	178.1 (9)
O1—Re3—O3	73.8 (2)	O13—C13—Re1	177.2 (8)
C32—Re3—O4	173.6 (3)	C105—N1—C101	117.7 (8)
C31—Re3—O4	99.9 (3)	C205—N2—C201	117.8 (9)
C33—Re3—O4	94.5 (3)	C305—N3—C301	117.7 (9)
O1—Re3—O4	75.0 (2)	C401—N4—C405	117.5 (9)
O3—Re3—O4	73.9 (2)	N3—C305—C304	124.5 (11)
C43—Re4—C42	87.2 (4)	N3—C305—H305	117.8
C43—Re4—C41	90.3 (4)	C304—C305—H305	117.8
C42—Re4—C41	88.4 (4)	C303—C302—C301	119.8 (12)
C43—Re4—O2	170.3 (3)	C303—C302—H302	120.1
C42—Re4—O2	98.0 (3)	C301—C302—H302	120.1
C41—Re4—O2	98.0 (3)	C303—C304—C305	117.5 (11)
C43—Re4—O3	97.0 (3)	C303—C304—H304	121.3
C42—Re4—O3	99.2 (3)	C305—C304—H304	121.3
C41—Re4—O3	169.6 (3)	C302—C303—C304	118.9 (11)
O2—Re4—O3	74.1 (2)	C302—C303—H303	120.6
C43—Re4—O4	100.4 (3)	C304—C303—H303	120.6
C42—Re4—O4	170.3 (3)	N3—C301—C302	121.6 (11)
C41—Re4—O4	97.5 (3)	N3—C301—H301	119.2
O2—Re4—O4	73.7 (2)	C302—C301—H301	119.2
O3—Re4—O4	74.0 (2)	C402—C403—C404	119.0 (9)
C23—Re2—C22	86.9 (4)	C402—C403—H403	120.5
C23—Re2—C21	89.0 (4)	C404—C403—H403	120.5
C22—Re2—C21	89.2 (4)	C403—C402—C401	119.7 (9)
C23—Re2—O3	170.2 (3)	C403—C402—H402	120.2
C22—Re2—O3	98.7 (3)	C401—C402—H402	120.2
C21—Re2—O3	99.0 (3)	N4—C401—C402	122.7 (9)
C23—Re2—O2	99.4 (3)	N4—C401—H401	118.7
C22—Re2—O2	170.9 (3)	C402—C401—H401	118.7
C21—Re2—O2	97.5 (3)	C403—C404—C405	118.3 (9)
O3—Re2—O2	74.2 (2)	C403—C404—H404	120.8
C23—Re2—O1	97.5 (3)	C405—C404—H404	120.8
C22—Re2—O1	99.0 (3)	N4—C405—C404	122.8 (9)
C21—Re2—O1	169.8 (3)	N4—C405—H405	118.6
O3—Re2—O1	73.8 (2)	C404—C405—H405	118.6
O2—Re2—O1	73.8 (2)	N2—C205—C204	122.5 (12)
Re3—O1—Re2	104.3 (2)	N2—C205—H205	118.8
Re3—O1—Re1	102.7 (3)	C204—C205—H205	118.8
Re2—O1—Re1	104.2 (2)	N2—C201—C202	122.7 (13)
Re3—O1—H1	118 (10)	N2—C201—H201	118.6
Re2—O1—H1	117 (10)	C202—C201—H201	118.6
Re1—O1—H1	108 (10)	C203—C204—C205	119.4 (13)
O23—C23—Re2	178.7 (8)	C203—C204—H204	120.3
Re1—O4—Re4	104.2 (3)	C205—C204—H204	120.3
Re1—O4—Re3	102.6 (3)	C202—C203—C204	118.3 (11)
Re4—O4—Re3	104.0 (2)	C202—C203—H203	120.9
Re1—O4—H4	117 (10)	C204—C203—H203	120.9
Re4—O4—H4	112 (10)	C203—C202—C201	119.3 (13)
Re3—O4—H4	116 (10)	C203—C202—H202	120.3
C12—Re1—C13	88.7 (4)	C201—C202—H202	120.3
C12—Re1—C11	88.4 (4)	N1—C105—C104	123.2 (9)
C13—Re1—C11	89.0 (4)	N1—C105—H105	118.4
C12—Re1—O4	97.2 (3)	C104—C105—H105	118.4
C13—Re1—O4	170.0 (3)	C104—C103—C102	118.7 (9)
C11—Re1—O4	99.1 (3)	C104—C103—H103	120.7
C12—Re1—O2	169.5 (3)	C102—C103—H103	120.7
C13—Re1—O2	99.5 (3)	C103—C104—C105	118.6 (9)
C11—Re1—O2	98.2 (4)	C103—C104—H104	120.7
O4—Re1—O2	73.7 (2)	C105—C104—H104	120.7
C12—Re1—O1	99.2 (3)	C101—C102—C103	119.1 (9)
C13—Re1—O1	96.2 (3)	C101—C102—H102	120.5
C11—Re1—O1	170.8 (3)	C103—C102—H102	120.5
O4—Re1—O1	75.0 (2)	N1—C101—C102	122.8 (9)
O2—Re1—O1	73.5 (2)	N1—C101—H101	118.6
Re2—O3—Re3	104.4 (2)	C102—C101—H101	118.6
Re2—O3—Re4	103.2 (2)	Re4—O2—Re2	103.5 (3)
Re3—O3—Re4	104.4 (2)	Re4—O2—Re1	104.6 (3)
Re2—O3—H3	112 (10)	Re2—O2—Re1	104.7 (2)
Re3—O3—H3	123 (10)	Re4—O2—H2	114 (8)
Re4—O3—H3	107 (10)	Re2—O2—H2	115 (8)
O43—C43—Re4	177.6 (8)	Re1—O2—H2	113 (7)

D—H···A	D—H	H···A	D···A	D—H···A
C103—H103···O23i	0.93	2.59	3.249 (12)	128
C203—H203···O33ii	0.93	2.42	3.330 (13)	166
C303—H303···O42iii	0.93	2.49	3.321 (13)	149
C404—H404···O32iv	0.93	2.47	3.252 (12)	142
O1—H1···N2	0.85 (2)	1.76 (4)	2.600 (10)	170 (16)
O2—H2···N3	0.85 (2)	1.74 (3)	2.586 (10)	174 (11)
O3—H3···N1	0.85 (2)	1.79 (4)	2.627 (10)	165 (14)
O4—H4···N4	0.85 (2)	1.78 (4)	2.620 (10)	169 (15)

Table 1

Selected bond lengths (Å)

Re3—C32	1.886 (10)
Re3—C31	1.900 (9)
Re3—C33	1.906 (10)
Re3—O1	2.157 (6)
Re3—O3	2.168 (6)
Re3—O4	2.179 (6)
Re4—C43	1.893 (9)
Re4—C42	1.913 (10)
Re4—C41	1.918 (9)
Re4—O2	2.154 (7)
Re4—O3	2.172 (6)
Re4—O4	2.173 (6)
Re2—C23	1.891 (9)
Re2—C22	1.916 (9)
Re2—C21	1.918 (10)
Re2—O3	2.157 (6)
Re2—O2	2.165 (6)
Re2—O1	2.171 (6)
O1—Re1	2.178 (6)
O4—Re1	2.160 (6)
Re1—C12	1.888 (10)
Re1—C13	1.889 (10)
Re1—C11	1.907 (10)
Re1—O2	2.169 (6)

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C103—H103⋯O23i	0.93	2.59	3.249 (12)	128
C203—H203⋯O33ii	0.93	2.42	3.330 (13)	166
C303—H303⋯O42iii	0.93	2.49	3.321 (13)	149
C404—H404⋯O32iv	0.93	2.47	3.252 (12)	142
O1—H1⋯N2	0.85 (2)	1.76 (4)	2.600 (10)	170 (16)
O2—H2⋯N3	0.85 (2)	1.74 (3)	2.586 (10)	174 (11)
O3—H3⋯N1	0.85 (2)	1.79 (4)	2.627 (10)	165 (14)
O4—H4⋯N4	0.85 (2)	1.78 (4)	2.620 (10)	169 (15)

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