fac-Bipyridyl­tri­carbonyl­(pyridine)­rhenium(I) tri­fluoro­methane­sulfonate

The structure of the title compound, [Re(C₅H₅N)(C₁₀H₈N₂)(CO)₃](CF₃O₃S), an emissive mol­ecule, shows the Re centre in the cation to be in a distorted octahedral geometry with a facial disposition of carbonyl ligands.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.011 Å
• R factor = 0.033
• wR factor = 0.074
• Data-to-parameter ratio = 12.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT052_ALERT_1_A (Proper) Absorption Correction Method Missing ..          ?
PLAT057_ALERT_3_A Correction for Absorption Required   RT(exp) ...       1.77

Alert level C
ABSTM02_ALERT_3_C  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
            Tmin and Tmax reported:      0.505     0.612
            Tmin and Tmax expected:      0.345     0.614
            RR =      1.468
            Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         11
PLAT431_ALERT_2_C Short Inter HL..A Contact  F2     ..  O2      ..       2.87 Ang.
PLAT431_ALERT_2_C Short Inter HL..A Contact  F2     ..  O1      ..       2.92 Ang.
PLAT712_ALERT_1_C ANGLE   Unknown or Inconsistent Label ..........        RE1
                    C13    N2     RE1

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

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994).; cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995).; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997).; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997).; software used to prepare material for publication: WinGX (Farrugia, 1999)..

(I)

Crystal data

[Re(C5H5N)(C10H8N2)(CO)3](CF3O3S)	F(000) = 2512
Mr = 654.58	Dx = 2.121 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -p 2ac 2ab	Cell parameters from 24 reflections
a = 12.178 (2) Å	θ = 10–12°
b = 14.414 (3) Å	µ = 6.10 mm^−1
c = 23.357 (5) Å	T = 100 K
V = 4100.1 (14) Å^3	Needle, green–yellow
Z = 8	0.38 × 0.15 × 0.08 mm

Data collection

Enraf–Nonius CAD-4 diffractometer	Rint = 0
non–profiled ω/2θ scans	θmax = 25.0°, θmin = 1.7°
Absorption correction: ψ scan North, Phillips & Mathews (1968)	h = 0→14
Tmin = 0.505, Tmax = 0.612	k = 0→17
3601 measured reflections	l = 0→27
3601 independent reflections	3 standard reflections every 60 min
2357 reflections with I > 2σ(I)	intensity decay: none

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.033	w = 1/[σ^2(Fo^2) + (0.0313P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.074	(Δ/σ)max = 0.001
S = 1.03	Δρmax = 1.01 e Å^−3
3601 reflections	Δρmin = −0.74 e Å^−3
298 parameters

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Re	0.237095 (18)	0.828579 (19)	0.334964 (11)	0.01160 (9)
S1	0.26244 (16)	0.28566 (13)	0.57860 (8)	0.0184 (4)
O1	0.0372 (4)	0.8173 (4)	0.2555 (2)	0.0219 (12)
O3	0.1465 (4)	0.6677 (4)	0.4072 (2)	0.0218 (12)
O4	0.2120 (5)	0.3763 (4)	0.5805 (2)	0.0300 (15)
N3	0.1639 (5)	0.9390 (4)	0.3872 (3)	0.0128 (15)
O2	0.3528 (4)	0.6731 (4)	0.2679 (2)	0.0188 (11)
N1	0.3817 (5)	0.8712 (5)	0.3828 (3)	0.0162 (15)
N2	0.3093 (5)	0.9400 (4)	0.2860 (2)	0.0124 (14)
F3	0.1897 (4)	0.1221 (4)	0.6089 (2)	0.0414 (15)
F2	0.1277 (4)	0.2342 (4)	0.6595 (2)	0.0520 (16)
C2	0.3099 (6)	0.7327 (6)	0.2926 (3)	0.0149 (17)
C4	0.4135 (6)	0.8308 (6)	0.4329 (3)	0.0177 (16)
H4	0.3735	0.779	0.4469	0.021*
C3	0.1806 (6)	0.7301 (6)	0.3812 (3)	0.0154 (17)
F1	0.0652 (4)	0.2120 (4)	0.5745 (2)	0.0399 (14)
C6	0.5590 (6)	0.9394 (6)	0.4443 (4)	0.0197 (19)
H6	0.6201	0.9629	0.4651	0.024*
C19	0.1559 (7)	0.2103 (7)	0.6066 (4)	0.027 (2)
C13	0.2729 (6)	0.9680 (5)	0.2347 (3)	0.0171 (16)
H13	0.2149	0.9348	0.2169	0.021*
C1	0.1101 (6)	0.8187 (6)	0.2860 (3)	0.0178 (17)
C15	0.1378 (6)	1.0102 (6)	0.4792 (3)	0.0198 (18)
H15	0.151	1.0094	0.5193	0.024*
C18	0.1082 (5)	1.0103 (6)	0.3650 (3)	0.0177 (18)
H18	0.0977	1.0112	0.3247	0.021*
C14	0.1770 (6)	0.9395 (5)	0.4448 (3)	0.0180 (18)
H14	0.2147	0.8893	0.4623	0.022*
C16	0.0798 (6)	1.0814 (6)	0.4550 (3)	0.0204 (19)
H16	0.0502	1.1293	0.4783	0.025*
C9	0.3956 (6)	0.9841 (6)	0.3100 (3)	0.0187 (18)
C8	0.4369 (6)	0.9447 (6)	0.3642 (4)	0.0177 (19)
C7	0.5254 (6)	0.9813 (6)	0.3935 (3)	0.0207 (18)
H7	0.5628	1.0344	0.3793	0.025*
C5	0.5021 (6)	0.8632 (6)	0.4639 (3)	0.0222 (19)
H5	0.5236	0.8332	0.4984	0.027*
C10	0.4414 (6)	1.0616 (5)	0.2839 (3)	0.0180 (18)
H10	0.5002	1.0937	0.3019	0.022*
C12	0.3172 (6)	1.0436 (5)	0.2071 (3)	0.0165 (17)
H12	0.2892	1.0622	0.1709	0.02*
C11	0.4014 (7)	1.0919 (5)	0.2318 (3)	0.023 (2)
H11	0.4317	1.145	0.2136	0.028*
C17	0.0646 (6)	1.0831 (6)	0.3965 (4)	0.0200 (18)
H17	0.0258	1.1323	0.3784	0.024*
O6	0.3522 (4)	0.2732 (4)	0.6177 (2)	0.0257 (14)
O5	0.2795 (4)	0.2492 (4)	0.5216 (2)	0.0254 (13)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re	0.01091 (13)	0.01109 (14)	0.01280 (14)	−0.00084 (13)	0.00098 (13)	0.00042 (15)
S1	0.0191 (10)	0.0175 (9)	0.0188 (9)	0.0016 (9)	0.0023 (9)	−0.0019 (8)
O1	0.015 (3)	0.025 (3)	0.025 (3)	−0.009 (2)	−0.006 (2)	−0.002 (3)
O3	0.027 (3)	0.019 (3)	0.019 (3)	−0.005 (3)	0.002 (2)	−0.003 (3)
O4	0.031 (3)	0.024 (3)	0.035 (4)	0.007 (3)	−0.005 (3)	−0.007 (3)
N3	0.013 (3)	0.014 (4)	0.012 (4)	0.002 (3)	−0.002 (3)	0.000 (3)
O2	0.019 (3)	0.018 (3)	0.018 (3)	0.006 (3)	0.003 (2)	−0.001 (3)
N1	0.012 (3)	0.019 (4)	0.017 (4)	0.008 (3)	0.001 (3)	−0.005 (3)
N2	0.014 (3)	0.014 (4)	0.009 (3)	−0.003 (3)	0.004 (3)	−0.002 (3)
F3	0.059 (4)	0.030 (3)	0.035 (3)	−0.014 (3)	−0.003 (3)	0.011 (3)
F2	0.060 (3)	0.075 (5)	0.021 (3)	−0.022 (3)	0.024 (3)	−0.016 (3)
C2	0.012 (4)	0.020 (5)	0.013 (4)	−0.005 (3)	−0.001 (3)	0.008 (4)
C4	0.018 (4)	0.021 (4)	0.015 (4)	0.007 (4)	0.001 (3)	−0.007 (4)
C3	0.016 (4)	0.013 (4)	0.017 (4)	0.002 (3)	0.007 (3)	−0.001 (4)
F1	0.025 (3)	0.055 (4)	0.040 (3)	−0.006 (2)	0.001 (2)	−0.010 (3)
C6	0.005 (3)	0.027 (5)	0.028 (5)	0.000 (3)	−0.004 (3)	−0.003 (4)
C19	0.030 (5)	0.037 (6)	0.015 (5)	−0.004 (4)	0.003 (4)	−0.005 (4)
C13	0.020 (4)	0.011 (4)	0.021 (4)	−0.002 (3)	0.002 (3)	−0.001 (3)
C1	0.009 (3)	0.017 (4)	0.027 (5)	0.001 (3)	0.006 (3)	−0.002 (4)
C15	0.022 (4)	0.026 (5)	0.011 (4)	−0.001 (4)	0.003 (3)	−0.004 (4)
C18	0.012 (4)	0.020 (5)	0.021 (5)	−0.002 (3)	−0.006 (3)	0.002 (4)
C14	0.024 (4)	0.014 (5)	0.017 (4)	0.003 (3)	0.006 (3)	0.001 (4)
C16	0.022 (4)	0.022 (5)	0.017 (4)	−0.002 (4)	0.007 (3)	−0.011 (4)
C9	0.018 (4)	0.018 (5)	0.021 (4)	0.004 (3)	0.003 (3)	0.002 (4)
C8	0.009 (4)	0.019 (5)	0.025 (5)	−0.006 (3)	0.003 (3)	0.000 (4)
C7	0.022 (4)	0.019 (5)	0.021 (4)	0.001 (4)	0.006 (3)	−0.005 (4)
C5	0.018 (4)	0.024 (5)	0.024 (5)	0.015 (3)	−0.003 (3)	−0.001 (4)
C10	0.020 (4)	0.014 (4)	0.020 (5)	−0.005 (3)	0.007 (3)	−0.001 (4)
C12	0.021 (4)	0.017 (4)	0.012 (4)	0.004 (3)	0.005 (3)	0.000 (3)
C11	0.035 (5)	0.007 (4)	0.027 (5)	0.000 (3)	0.012 (4)	0.000 (4)
C17	0.022 (4)	0.011 (4)	0.028 (5)	−0.001 (3)	0.004 (4)	−0.001 (4)
O6	0.015 (3)	0.030 (4)	0.032 (4)	0.001 (2)	−0.009 (2)	−0.004 (3)
O5	0.036 (3)	0.027 (3)	0.014 (3)	0.001 (3)	0.007 (2)	−0.003 (3)

Geometric parameters (Å, º)

Re—N1	2.174 (6)	C6—C5	1.377 (11)
Re—N2	2.158 (6)	C6—C7	1.393 (11)
Re—N3	2.194 (6)	C6—H6	0.95
Re—C1	1.929 (7)	C13—C12	1.375 (10)
Re—C2	1.918 (8)	C13—H13	0.95
Re—C3	1.912 (8)	C15—C16	1.368 (11)
S1—O6	1.435 (5)	C15—C14	1.382 (10)
S1—O4	1.444 (6)	C15—H15	0.95
S1—O5	1.446 (5)	C18—C17	1.387 (11)
S1—C19	1.815 (9)	C18—H18	0.95
O1—C1	1.139 (9)	C14—H14	0.95
O3—C3	1.162 (9)	C16—C17	1.380 (11)
N3—C18	1.335 (9)	C16—H16	0.95
N3—C14	1.357 (9)	C9—C10	1.390 (11)
O2—C2	1.158 (9)	C9—C8	1.476 (11)
N1—C8	1.328 (10)	C8—C7	1.382 (11)
N1—C4	1.362 (9)	C7—H7	0.95
N2—C13	1.341 (9)	C5—H5	0.95
N2—C9	1.349 (9)	C10—C11	1.383 (11)
F3—C19	1.337 (11)	C10—H10	0.95
F2—C19	1.327 (9)	C12—C11	1.368 (11)
C4—C5	1.381 (10)	C12—H12	0.95
C4—H4	0.95	C11—H11	0.95
F1—C19	1.335 (10)	C17—H17	0.95
N1—Re—N2	74.5 (2)	F1—C19—S1	112.2 (6)
N1—Re—N3	80.7 (2)	F3—C19—S1	111.3 (6)
N1—Re—C1	167.2 (3)	N2—C13—C12	121.9 (7)
N1—Re—C2	95.4 (3)	N2—C13—H13	119
N1—Re—C3	102.2 (3)	C12—C13—H13	119
N2—Re—N3	85.4 (2)	O1—C1—Re	176.1 (7)
N2—Re—C1	93.9 (3)	C16—C15—C14	119.5 (7)
N2—Re—C2	94.3 (2)	C16—C15—H15	120.3
N2—Re—C3	176.6 (3)	C14—C15—H15	120.3
N3—Re—C1	93.3 (3)	N3—C18—C17	124.9 (8)
N3—Re—C2	176.1 (3)	N3—C18—H18	117.5
N3—Re—C3	94.5 (3)	C17—C18—H18	117.5
C1—Re—C2	90.7 (3)	N3—C14—C15	122.7 (7)
C1—Re—C3	89.5 (3)	N3—C14—H14	118.7
C2—Re—C3	85.6 (3)	C15—C14—H14	118.7
O6—S1—O4	114.7 (4)	C15—C16—C17	119.4 (8)
O6—S1—O5	115.5 (3)	C15—C16—H16	120.3
O4—S1—O5	114.7 (3)	C17—C16—H16	120.3
O6—S1—C19	103.9 (4)	N2—C9—C10	120.6 (7)
O4—S1—C19	103.1 (4)	N2—C9—C8	116.1 (7)
O5—S1—C19	102.5 (4)	C10—C9—C8	123.3 (7)
C18—N3—C14	116.1 (7)	N1—C8—C7	122.5 (8)
C18—N3—Re	123.3 (5)	N1—C8—C9	114.5 (7)
C14—N3—Re	120.5 (5)	C7—C8—C9	122.9 (7)
C8—N1—C4	118.5 (7)	C8—C7—C6	119.0 (8)
C8—N1—Re	117.9 (5)	C8—C7—H7	120.5
C4—N1—Re	123.4 (5)	C6—C7—H7	120.5
C13—N2—C9	119.1 (6)	C6—C5—C4	119.2 (8)
C13—N2—Re1	124.3 (5)	C6—C5—H5	120.4
C9—N2—Re	116.6 (5)	C4—C5—H5	120.4
O2—C2—Re	178.3 (7)	C11—C10—C9	119.9 (8)
N1—C4—C5	121.9 (8)	C11—C10—H10	120
N1—C4—H4	119	C9—C10—H10	120
C5—C4—H4	119	C11—C12—C13	120.0 (7)
O3—C3—Re	176.9 (7)	C11—C12—H12	120
C5—C6—C7	118.8 (7)	C13—C12—H12	120
C5—C6—H6	120.6	C12—C11—C10	118.3 (7)
C7—C6—H6	120.6	C12—C11—H11	120.8
F2—C19—F1	107.7 (7)	C10—C11—H11	120.8
F2—C19—F3	106.9 (8)	C16—C17—C18	117.4 (8)
F1—C19—F3	107.1 (7)	C16—C17—H17	121.3
F2—C19—S1	111.4 (6)	C18—C17—H17	121.3