Crystal structure of tricarbon-yltris(pyri-dine-κN)rhenium(I) tetra-fluorido-borate.

In the title compound, [Re(C6H5N)3(CO)3]BF4, the Re(I) ion is six-coordinated by three pyridine N atoms and three carbonyl C atoms. In each case, the carbonyl C atom lies trans to a pyridine N atom. In the crystal, the ions are linked via C-H⋯F hydrogen bonds and C-H⋯π inter-actions, forming a three-dimensional framework. The F atoms of the BF4 anion are disordered over two positions and gave a final refined occupancy ratio of 0.705 (11):0.295 (11).

Related literature

For background to rhenium tricarbonyl complexes, see: Amoroso et al. (2008 ▸); Coogan et al. (2009 ▸). For the structure of tricarbonyl tris-pyridyl rhenium(I) hexa­fluoro­phosphate, see: Franklin et al. (2008 ▸). For the preparation of [Re(C14H10N2O)(CO)3Br] used in the synthesis, see: Al Subari et al. (2010 ▸); Coogan et al. (2009 ▸).

Experimental

Crystal data

[Re(C6H5N)3(CO)3]BF4

M = 594.34

Monoclinic,

a = 8.1272 (12) Å

b = 18.718 (3) Å

c = 13.046 (2) Å

β = 97.317 (9)°

V = 1968.5 (5) Å3

Z = 4

Cu Kα radiation

μ = 12.66 mm−1

T = 110 K

0.08 × 0.06 × 0.02 mm

Data collection

Bruker GADDS D8 Discover diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2006 ▸) T min = 0.431, T max = 0.786

39315 measured reflections

2891 independent reflections

2589 reflections with I > 2σ(I)

R int = 0.052

θmax = 60.0°

Standard reflections: 0

Refinement

R[F 2 > 2σ(F 2)] = 0.023

wR(F 2) = 0.048

S = 1.11

2891 reflections

308 parameters

172 restraints

H-atom parameters constrained

Δρmax = 0.98 e Å−3

Δρmin = −0.98 e Å−3

Data collection: APEX2 and FRAMBO (Bruker, 2004 ▸); cell refinement: SAINT (Bruker, 2004 ▸); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▸); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▸); molecular graphics: X-SEED (Barbour, 2001 ▸); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▸) and PLATON (Spek, 2009 ▸).

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989015006180/su5093sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989015006180/su5093Isup2.hkl

Click here for additional data file.

. DOI: 10.1107/S2056989015006180/su5093fig1.tif

The mol­ecular structure of the title compound, with atom labelling. Displacement ellipsoids are drawn at the 50% probability level.

Click here for additional data file.

. DOI: 10.1107/S2056989015006180/su5093fig2.tif

Preparation of the title compound.

CCDC reference: 1022851

Additional supporting information: crystallographic information; 3D view; checkCIF report

[Re(C6H5N)3(CO)3]BF4	F(000) = 1136
Mr = 594.34	Dx = 2.005 Mg m−3
Monoclinic, P21/c	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: P 2ybc	Cell parameters from 2921 reflections
a = 8.1272 (12) Å	θ = 4.2–62.4°
b = 18.718 (3) Å	µ = 12.66 mm−1
c = 13.046 (2) Å	T = 110 K
β = 97.317 (9)°	Block, colourless
V = 1968.5 (5) Å3	0.08 × 0.06 × 0.02 mm
Z = 4

Bruker GADDS D8 Discover diffractometer	2891 independent reflections
Radiation source: fine-focus sealed tube	2589 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.052
phi and ω scans	θmax = 60.0°, θmin = 4.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 2006)	h = −9→9
Tmin = 0.431, Tmax = 0.786	k = −21→21
39315 measured reflections	l = −14→14

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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.048	H-atom parameters constrained
S = 1.11	w = 1/[σ2(Fo2) + (0.0131P)2 + 6.6179P] where P = (Fo2 + 2Fc2)/3
2891 reflections	(Δ/σ)max = 0.001
308 parameters	Δρmax = 0.98 e Å−3
172 restraints	Δρmin = −0.98 e Å−3

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.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Re1	0.90696 (2)	0.817237 (10)	0.800171 (15)	0.01465 (7)
C1	1.1344 (6)	0.8090 (2)	0.8614 (3)	0.0212 (10)
C2	0.9740 (5)	0.9040 (2)	0.7377 (3)	0.0188 (10)
C3	0.9626 (5)	0.7679 (2)	0.6806 (4)	0.0187 (10)
C4	0.5751 (6)	0.8920 (2)	0.7123 (3)	0.0209 (10)
H4A	0.6364	0.9327	0.7387	0.025*
C5	0.4181 (6)	0.9021 (3)	0.6613 (4)	0.0235 (10)
H5A	0.3714	0.9486	0.6534	0.028*
C6	0.3314 (6)	0.8441 (3)	0.6224 (4)	0.0253 (10)
H6A	0.2237	0.8500	0.5857	0.030*
C7	0.3993 (6)	0.7762 (3)	0.6360 (4)	0.0255 (11)
H7A	0.3388	0.7352	0.6100	0.031*
C8	0.5569 (5)	0.7699 (2)	0.6884 (3)	0.0190 (10)
H8A	0.6045	0.7236	0.6978	0.023*
C9	0.7018 (6)	0.7040 (2)	0.9139 (3)	0.0223 (11)
H9A	0.6199	0.7405	0.9073	0.027*
C10	0.6690 (6)	0.6415 (2)	0.9644 (3)	0.0226 (11)
H10A	0.5663	0.6355	0.9910	0.027*
C11	0.7859 (6)	0.5882 (2)	0.9758 (4)	0.0255 (11)
H11A	0.7674	0.5452	1.0112	0.031*
C12	0.9321 (6)	0.5994 (2)	0.9336 (4)	0.0246 (11)
H12A	1.0154	0.5635	0.9392	0.030*
C13	0.9560 (6)	0.6625 (2)	0.8837 (4)	0.0221 (11)
H13A	1.0565	0.6691	0.8548	0.027*
C14	0.6690 (6)	0.8790 (2)	0.9558 (4)	0.0233 (11)
H14A	0.5847	0.8586	0.9074	0.028*
C15	0.6234 (6)	0.9127 (3)	1.0420 (4)	0.0289 (12)
H15A	0.5100	0.9150	1.0526	0.035*
C16	0.7436 (6)	0.9430 (3)	1.1123 (4)	0.0295 (12)
H16A	0.7151	0.9666	1.1720	0.035*
C17	0.9070 (6)	0.9383 (2)	1.0939 (4)	0.0264 (11)
H17A	0.9930	0.9586	1.1412	0.032*
C18	0.9439 (6)	0.9040 (2)	1.0070 (4)	0.0217 (10)
H18A	1.0567	0.9014	0.9952	0.026*
N1	0.6466 (4)	0.82675 (18)	0.7269 (3)	0.0160 (8)
N2	0.8427 (4)	0.71536 (18)	0.8741 (3)	0.0173 (8)
N3	0.8279 (4)	0.87363 (19)	0.9373 (3)	0.0179 (8)
O1	1.2715 (4)	0.80628 (18)	0.8956 (3)	0.0309 (8)
O2	1.0248 (4)	0.95285 (17)	0.6991 (2)	0.0273 (8)
O3	0.9949 (4)	0.74082 (17)	0.6064 (2)	0.0255 (7)
B1	0.3395 (7)	0.5865 (3)	0.7653 (5)	0.0338 (14)	0.705 (11)
F1	0.5081 (9)	0.5915 (5)	0.7637 (9)	0.056 (3)	0.705 (11)
F2	0.3088 (9)	0.5538 (3)	0.8585 (5)	0.0468 (17)	0.705 (11)
F3	0.2785 (6)	0.5397 (3)	0.6835 (4)	0.0522 (18)	0.705 (11)
F4	0.2648 (13)	0.6503 (3)	0.7527 (8)	0.082 (3)	0.705 (11)
B1A	0.3395 (7)	0.5865 (3)	0.7653 (5)	0.0338 (14)	0.295 (11)
F1A	0.5017 (19)	0.5630 (8)	0.776 (2)	0.026 (4)	0.295 (11)
F2A	0.236 (2)	0.5462 (8)	0.8115 (18)	0.061 (5)	0.295 (11)
F3A	0.2854 (15)	0.5990 (11)	0.6583 (9)	0.069 (6)	0.295 (11)
F4A	0.3349 (16)	0.6580 (6)	0.8070 (12)	0.035 (3)	0.295 (11)

	U11	U22	U33	U12	U13	U23
Re1	0.01373 (11)	0.01449 (11)	0.01556 (11)	−0.00004 (9)	0.00123 (7)	−0.00028 (9)
C1	0.029 (3)	0.022 (2)	0.014 (2)	0.001 (2)	0.004 (2)	0.000 (2)
C2	0.014 (2)	0.022 (2)	0.019 (2)	0.003 (2)	−0.003 (2)	−0.007 (2)
C3	0.012 (2)	0.017 (2)	0.026 (3)	−0.0014 (18)	−0.001 (2)	0.008 (2)
C4	0.024 (3)	0.018 (2)	0.021 (3)	0.000 (2)	0.004 (2)	0.000 (2)
C5	0.020 (2)	0.028 (2)	0.024 (2)	0.0068 (19)	0.007 (2)	0.005 (2)
C6	0.015 (2)	0.032 (2)	0.027 (2)	−0.0113 (18)	−0.0049 (19)	0.005 (2)
C7	0.025 (3)	0.029 (2)	0.022 (2)	−0.010 (2)	−0.001 (2)	0.003 (2)
C8	0.022 (3)	0.017 (2)	0.017 (2)	−0.0016 (19)	0.001 (2)	0.000 (2)
C9	0.022 (3)	0.023 (2)	0.021 (3)	−0.001 (2)	0.001 (2)	−0.002 (2)
C10	0.026 (3)	0.023 (3)	0.020 (3)	−0.005 (2)	0.006 (2)	0.006 (2)
C11	0.037 (3)	0.019 (2)	0.021 (3)	−0.005 (2)	0.002 (2)	0.000 (2)
C12	0.029 (3)	0.016 (2)	0.027 (3)	0.004 (2)	−0.001 (2)	−0.002 (2)
C13	0.017 (2)	0.025 (3)	0.024 (3)	0.003 (2)	0.003 (2)	−0.004 (2)
C14	0.023 (3)	0.027 (3)	0.020 (3)	−0.005 (2)	0.002 (2)	0.000 (2)
C15	0.030 (3)	0.030 (3)	0.031 (3)	−0.001 (2)	0.015 (2)	−0.004 (2)
C16	0.036 (3)	0.027 (3)	0.028 (3)	−0.003 (2)	0.013 (2)	−0.012 (2)
C17	0.031 (3)	0.023 (3)	0.025 (3)	−0.008 (2)	0.000 (2)	−0.008 (2)
C18	0.021 (3)	0.018 (2)	0.025 (3)	−0.001 (2)	0.001 (2)	0.003 (2)
N1	0.0159 (19)	0.0144 (19)	0.0174 (19)	−0.0027 (15)	0.0015 (15)	0.0026 (16)
N2	0.020 (2)	0.0159 (18)	0.0159 (19)	0.0004 (16)	0.0010 (16)	−0.0024 (16)
N3	0.021 (2)	0.0170 (19)	0.015 (2)	−0.0008 (16)	0.0030 (17)	0.0034 (16)
O1	0.0159 (19)	0.042 (2)	0.033 (2)	0.0020 (15)	−0.0057 (16)	0.0022 (17)
O2	0.0305 (19)	0.0204 (17)	0.0315 (19)	−0.0066 (15)	0.0058 (16)	0.0017 (16)
O3	0.0288 (19)	0.0264 (18)	0.0222 (18)	−0.0004 (15)	0.0060 (15)	−0.0044 (16)
B1	0.025 (3)	0.031 (3)	0.048 (4)	−0.004 (3)	0.013 (3)	−0.005 (3)
F1	0.034 (3)	0.092 (8)	0.045 (5)	−0.021 (4)	0.014 (3)	−0.029 (6)
F2	0.045 (4)	0.035 (3)	0.063 (4)	−0.007 (3)	0.016 (3)	0.006 (3)
F3	0.044 (3)	0.043 (4)	0.062 (3)	−0.008 (2)	−0.019 (2)	0.001 (3)
F4	0.121 (7)	0.036 (3)	0.106 (7)	0.031 (4)	0.075 (6)	0.029 (4)
B1A	0.025 (3)	0.031 (3)	0.048 (4)	−0.004 (3)	0.013 (3)	−0.005 (3)
F1A	0.017 (5)	0.023 (8)	0.043 (8)	0.003 (5)	0.017 (5)	−0.001 (7)
F2A	0.031 (8)	0.032 (6)	0.130 (15)	−0.009 (6)	0.044 (9)	−0.002 (9)
F3A	0.038 (7)	0.111 (16)	0.054 (6)	0.018 (7)	−0.010 (5)	−0.010 (7)
F4A	0.028 (7)	0.017 (5)	0.059 (9)	0.009 (4)	0.001 (6)	0.009 (5)

Re1—C3	1.916 (5)	C10—C11	1.372 (7)
Re1—C1	1.924 (5)	C10—H10A	0.9500
Re1—C2	1.926 (5)	C11—C12	1.387 (7)
Re1—N1	2.215 (3)	C11—H11A	0.9500
Re1—N2	2.229 (4)	C12—C13	1.376 (6)
Re1—N3	2.240 (4)	C12—H12A	0.9500
C1—O1	1.148 (5)	C13—N2	1.346 (6)
C2—O2	1.146 (5)	C13—H13A	0.9500
C3—O3	1.152 (5)	C14—N3	1.348 (6)
C4—N1	1.355 (6)	C14—C15	1.381 (7)
C4—C5	1.375 (6)	C14—H14A	0.9500
C4—H4A	0.9500	C15—C16	1.375 (7)
C5—C6	1.356 (7)	C15—H15A	0.9500
C5—H5A	0.9500	C16—C17	1.382 (7)
C6—C7	1.389 (7)	C16—H16A	0.9500
C6—H6A	0.9500	C17—C18	1.369 (7)
C7—C8	1.378 (6)	C17—H17A	0.9500
C7—H7A	0.9500	C18—N3	1.349 (6)
C8—N1	1.350 (5)	C18—H18A	0.9500
C8—H8A	0.9500	B1—F4	1.340 (8)
C9—N2	1.334 (6)	B1—F1	1.376 (9)
C9—C10	1.385 (6)	B1—F2	1.412 (8)
C9—H9A	0.9500	B1—F3	1.420 (7)
C3—Re1—C1	89.17 (18)	C10—C11—C12	117.7 (4)
C3—Re1—C2	87.34 (18)	C10—C11—H11A	121.2
C1—Re1—C2	86.22 (18)	C12—C11—H11A	121.2
C3—Re1—N1	89.95 (16)	C13—C12—C11	119.8 (4)
C1—Re1—N1	178.97 (16)	C13—C12—H12A	120.1
C2—Re1—N1	93.21 (15)	C11—C12—H12A	120.1
C3—Re1—N2	91.85 (15)	N2—C13—C12	122.6 (4)
C1—Re1—N2	91.02 (16)	N2—C13—H13A	118.7
C2—Re1—N2	177.13 (16)	C12—C13—H13A	118.7
N1—Re1—N2	89.54 (13)	N3—C14—C15	122.9 (4)
C3—Re1—N3	176.99 (16)	N3—C14—H14A	118.6
C1—Re1—N3	93.69 (16)	C15—C14—H14A	118.6
C2—Re1—N3	93.77 (16)	C16—C15—C14	119.3 (5)
N1—Re1—N3	87.20 (13)	C16—C15—H15A	120.3
N2—Re1—N3	87.18 (12)	C14—C15—H15A	120.3
O1—C1—Re1	177.4 (4)	C15—C16—C17	118.4 (4)
O2—C2—Re1	174.7 (4)	C15—C16—H16A	120.8
O3—C3—Re1	177.1 (4)	C17—C16—H16A	120.8
N1—C4—C5	123.2 (4)	C18—C17—C16	119.3 (4)
N1—C4—H4A	118.4	C18—C17—H17A	120.3
C5—C4—H4A	118.4	C16—C17—H17A	120.3
C6—C5—C4	118.4 (4)	N3—C18—C17	123.3 (4)
C6—C5—H5A	120.8	N3—C18—H18A	118.4
C4—C5—H5A	120.8	C17—C18—H18A	118.4
C5—C6—C7	120.4 (4)	C8—N1—C4	117.1 (4)
C5—C6—H6A	119.8	C8—N1—Re1	122.6 (3)
C7—C6—H6A	119.8	C4—N1—Re1	120.1 (3)
C8—C7—C6	118.1 (4)	C9—N2—C13	117.2 (4)
C8—C7—H7A	121.0	C9—N2—Re1	124.4 (3)
C6—C7—H7A	121.0	C13—N2—Re1	118.3 (3)
N1—C8—C7	122.8 (4)	C14—N3—C18	116.8 (4)
N1—C8—H8A	118.6	C14—N3—Re1	123.9 (3)
C7—C8—H8A	118.6	C18—N3—Re1	119.4 (3)
N2—C9—C10	123.2 (4)	F4—B1—F1	112.0 (6)
N2—C9—H9A	118.4	F4—B1—F2	111.4 (6)
C10—C9—H9A	118.4	F1—B1—F2	109.1 (7)
C11—C10—C9	119.5 (4)	F4—B1—F3	110.4 (7)
C11—C10—H10A	120.3	F1—B1—F3	106.5 (6)
C9—C10—H10A	120.3	F2—B1—F3	107.2 (5)

D—H···A	D—H	H···A	D···A	D—H···A
C4—H4A···F3i	0.95	2.31	3.240 (7)	165
C13—H13A···F4ii	0.95	2.31	3.219 (12)	160
C17—H17A···F3iii	0.95	2.32	3.123 (7)	142
C10—H10A···Cg1iv	0.95	2.61	3.302 (5)	130

Table 1

Selected bond lengths ()

Re1C3	1.916(5)
Re1C1	1.924(5)
Re1C2	1.926(5)
Re1N1	2.215(3)
Re1N2	2.229(4)
Re1N3	2.240(4)

Table 2

Hydrogen-bond geometry (, )

Cg1 is the centroid of the N1/C4C8 pyrdine ring.

DHA	DH	HA	D A	DHA
C4H4AF3i	0.95	2.31	3.240(7)	165
C13H13AF4ii	0.95	2.31	3.219(12)	160
C17H17AF3iii	0.95	2.32	3.123(7)	142
C10H10A Cg1iv	0.95	2.61	3.302(5)	130

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