(Acetonitrile)(2,2'-bipyridine)tricarbonyl­rhenium(I) perchlorate

The title compound, [Re(C₂H₃N)(C₁₀H₈N₂)(CO)₃]ClO₄, was isolated from the reaction between [ReCl(bpy)(CO)₃] (bpy is 2,2'-bipyridine) and AgClO₄ in acetonitrile. The Re atom adopts a distorted octahedral geometry.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.024
• wR factor = 0.061
• Data-to-parameter ratio = 16.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature         293
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Re     -   C21     ..       5.66 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Re     -   C41     ..       6.44 su
PLAT432_ALERT_2_C Short Inter X...Y Contact  O3     ..  C51     ..       2.96 Ang.

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

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

---

Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(Acetonitrile)(2,2'-bipyridine)tricarbonylrhenium(I) perchlorate

Crystal data

[Re(C2H3N)(C10H8N2)(CO)3]ClO4	F(000) = 2160
Mr = 566.92	Dx = 2.163 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 4993 reflections
a = 33.745 (5) Å	θ = 3.3–27.5°
b = 6.3132 (11) Å	µ = 7.18 mm^−1
c = 18.793 (4) Å	T = 293 K
β = 119.572 (10)°	Prism, yellow
V = 3482.1 (11) Å^3	0.55 × 0.40 × 0.30 mm
Z = 8

Data collection

Rigaku Mercury70 diffractometer	3966 independent reflections
Radiation source: Rotating anode	3745 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
Detector resolution: 14.6306 pixels mm^-1	θmax = 27.5°, θmin = 3.4°
CCD profile–fitting scans	h = −43→29
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −8→8
Tmin = 0.043, Tmax = 0.113	l = −24→23
12732 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.061	H-atom parameters constrained
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0365P)^2 + 5.548P] where P = (Fo^2 + 2Fc^2)/3
3966 reflections	(Δ/σ)max = 0.002
244 parameters	Δρmax = 2.50 e Å^−3
0 restraints	Δρmin = −2.45 e Å^−3

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.

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 (Ų)

	x	y	z	Uiso*/Ueq
Re	0.570648 (4)	1.058495 (18)	0.204326 (7)	0.01148 (6)
N1	0.63532 (9)	0.9050 (4)	0.23938 (16)	0.0125 (5)
N2	0.62202 (9)	1.2595 (4)	0.29842 (15)	0.0129 (5)
N3	0.58441 (9)	1.2290 (4)	0.12046 (16)	0.0159 (5)
C31	0.51723 (11)	1.2289 (5)	0.17478 (19)	0.0185 (7)
C12	0.64638 (13)	1.5612 (5)	0.3874 (2)	0.0174 (7)
H12A	0.6388	1.6836	0.4056	0.021*
C11	0.61268 (12)	1.4348 (5)	0.3279 (2)	0.0153 (6)
H11A	0.5824	1.4732	0.3076	0.018*
C41	0.55802 (11)	0.9139 (5)	0.2809 (2)	0.0156 (6)
C5	0.67384 (11)	1.0053 (5)	0.29561 (18)	0.0144 (6)
C14	0.70129 (11)	1.3182 (5)	0.39040 (19)	0.0173 (6)
H14A	0.7313	1.2743	0.4117	0.021*
C51	0.58895 (10)	1.3152 (5)	0.07203 (19)	0.0164 (6)
C15	0.66620 (10)	1.2005 (5)	0.32970 (18)	0.0140 (6)
C2	0.68122 (12)	0.6359 (5)	0.2259 (2)	0.0194 (7)
H2B	0.6828	0.5103	0.2016	0.023*
C3	0.72039 (12)	0.7379 (6)	0.2825 (2)	0.0211 (7)
H3B	0.7489	0.6826	0.2968	0.025*
C4	0.71649 (12)	0.9245 (5)	0.3179 (2)	0.0181 (7)
H4B	0.7425	0.9949	0.3564	0.022*
C1	0.63979 (11)	0.7240 (5)	0.20612 (19)	0.0169 (6)
H1B	0.6135	0.6550	0.1678	0.020*
C21	0.53262 (12)	0.8599 (6)	0.1205 (2)	0.0214 (7)
C13	0.69137 (12)	1.5016 (6)	0.4192 (2)	0.0188 (6)
H13A	0.7146	1.5831	0.4593	0.023*
C52	0.59441 (13)	1.4297 (6)	0.0105 (2)	0.0231 (8)
H52A	0.6174	1.5367	0.0365	0.028*
H52B	0.5660	1.4952	−0.0274	0.028*
H52C	0.6034	1.3330	−0.0183	0.028*
O41	0.54842 (8)	0.8296 (4)	0.32447 (14)	0.0208 (5)
O4	0.79882 (11)	0.5629 (4)	0.4817 (2)	0.0329 (7)
O31	0.48542 (9)	1.3297 (4)	0.15739 (16)	0.0294 (6)
O3	0.82798 (10)	0.5738 (4)	0.39152 (18)	0.0317 (7)
O2	0.81000 (9)	0.2461 (4)	0.42782 (16)	0.0258 (5)
O21	0.51093 (9)	0.7376 (5)	0.07130 (16)	0.0344 (6)
O1	0.87303 (11)	0.4419 (5)	0.5246 (2)	0.0430 (8)
Cl	0.82773 (3)	0.45588 (12)	0.45672 (5)	0.01887 (17)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re	0.00864 (8)	0.01332 (8)	0.01116 (8)	−0.00090 (4)	0.00386 (6)	0.00004 (4)
N1	0.0101 (13)	0.0149 (12)	0.0124 (12)	0.0004 (10)	0.0055 (11)	0.0009 (10)
N2	0.0130 (13)	0.0145 (12)	0.0124 (12)	−0.0010 (10)	0.0072 (10)	0.0009 (9)
N3	0.0138 (13)	0.0180 (13)	0.0141 (13)	−0.0005 (10)	0.0054 (11)	−0.0015 (10)
C31	0.0164 (16)	0.0215 (16)	0.0161 (15)	−0.0001 (13)	0.0070 (13)	0.0032 (12)
C12	0.0236 (18)	0.0161 (16)	0.0153 (16)	−0.0011 (12)	0.0117 (14)	−0.0022 (11)
C11	0.0153 (16)	0.0165 (16)	0.0157 (15)	−0.0006 (11)	0.0089 (13)	−0.0004 (11)
C41	0.0095 (15)	0.0171 (15)	0.0175 (15)	0.0036 (11)	0.0046 (13)	−0.0003 (12)
C5	0.0137 (15)	0.0161 (14)	0.0133 (14)	−0.0017 (13)	0.0067 (12)	0.0022 (12)
C14	0.0141 (15)	0.0203 (16)	0.0156 (14)	−0.0015 (12)	0.0060 (12)	−0.0020 (12)
C51	0.0121 (14)	0.0192 (15)	0.0141 (14)	0.0001 (12)	0.0036 (12)	−0.0031 (12)
C15	0.0145 (15)	0.0156 (15)	0.0121 (14)	−0.0001 (12)	0.0067 (12)	0.0007 (11)
C2	0.0262 (18)	0.0160 (16)	0.0191 (16)	0.0051 (13)	0.0135 (14)	0.0011 (12)
C3	0.0195 (17)	0.0254 (17)	0.0207 (16)	0.0037 (13)	0.0117 (14)	0.0020 (13)
C4	0.0128 (16)	0.0217 (17)	0.0179 (16)	0.0010 (12)	0.0061 (13)	0.0011 (12)
C1	0.0197 (16)	0.0160 (15)	0.0164 (15)	−0.0009 (12)	0.0099 (13)	−0.0016 (12)
C21	0.0182 (17)	0.0240 (18)	0.0212 (17)	−0.0028 (14)	0.0092 (14)	0.0000 (14)
C13	0.0206 (17)	0.0202 (15)	0.0144 (15)	−0.0068 (14)	0.0076 (13)	−0.0035 (13)
C52	0.0228 (19)	0.030 (2)	0.0172 (17)	−0.0033 (13)	0.0101 (15)	0.0030 (13)
O41	0.0166 (12)	0.0257 (13)	0.0208 (12)	0.0012 (10)	0.0097 (10)	0.0070 (10)
O4	0.0345 (17)	0.0297 (16)	0.0424 (17)	−0.0048 (11)	0.0250 (15)	−0.0137 (12)
O31	0.0206 (13)	0.0360 (15)	0.0303 (14)	0.0127 (12)	0.0115 (11)	0.0115 (12)
O3	0.0281 (16)	0.0344 (16)	0.0321 (15)	−0.0057 (11)	0.0145 (13)	0.0027 (11)
O2	0.0238 (13)	0.0248 (13)	0.0285 (13)	−0.0064 (10)	0.0128 (11)	−0.0098 (10)
O21	0.0268 (15)	0.0382 (16)	0.0298 (14)	−0.0130 (12)	0.0075 (12)	−0.0164 (12)
O1	0.0224 (16)	0.045 (2)	0.0344 (17)	−0.0021 (12)	−0.0070 (13)	−0.0014 (13)
Cl	0.0145 (4)	0.0203 (4)	0.0186 (4)	−0.0033 (3)	0.0057 (3)	−0.0043 (3)

Geometric parameters (Å, º)

Re—N1	2.172 (3)	C14—C13	1.387 (5)
Re—N2	2.172 (3)	C14—H14A	0.9300
Re—N3	2.140 (3)	C51—C52	1.451 (5)
Re—C21	1.925 (4)	C2—C1	1.374 (5)
Re—C31	1.931 (3)	C2—C3	1.380 (5)
Re—C41	1.921 (3)	C2—H2B	0.9300
N3—C51	1.133 (4)	C3—C4	1.391 (5)
N1—C1	1.346 (4)	C3—H3B	0.9300
N1—C5	1.361 (4)	C4—H4B	0.9300
N2—C11	1.343 (4)	C1—H1B	0.9300
N2—C15	1.357 (4)	C21—O21	1.148 (4)
C31—O31	1.148 (4)	C13—H13A	0.9300
C12—C13	1.381 (5)	C52—H52A	0.9600
C12—C11	1.387 (5)	C52—H52B	0.9600
C12—H12A	0.9300	C52—H52C	0.9600
C11—H11A	0.9300	O4—Cl	1.442 (3)
C41—O41	1.149 (4)	O3—Cl	1.437 (3)
C5—C4	1.383 (5)	O2—Cl	1.444 (3)
C5—C15	1.469 (4)	O1—Cl	1.431 (3)
C14—C15	1.386 (4)
N1—Re—N2	74.63 (10)	C15—C14—H14A	120.1
N1—Re—N3	84.08 (10)	C13—C14—H14A	120.1
N1—Re—C21	97.00 (13)	N3—C51—C52	178.7 (4)
N1—Re—C31	172.62 (12)	N2—C15—C14	121.3 (3)
N1—Re—C41	97.01 (12)	N2—C15—C5	115.7 (3)
N2—Re—N3	85.96 (10)	C14—C15—C5	123.1 (3)
N2—Re—C21	171.42 (13)	C1—C2—C3	118.6 (3)
N2—Re—C31	99.51 (12)	C1—C2—H2B	120.7
N2—Re—C41	92.92 (12)	C3—C2—H2B	120.7
N3—Re—C21	91.37 (13)	C2—C3—C4	118.9 (3)
N3—Re—C31	91.09 (12)	C2—C3—H3B	120.6
N3—Re—C41	178.18 (12)	C4—C3—H3B	120.6
C21—Re—C31	88.68 (15)	C5—C4—C3	119.9 (3)
C21—Re—C41	89.94 (14)	C5—C4—H4B	120.1
C31—Re—C41	87.68 (13)	C3—C4—H4B	120.1
C51—N3—Re	175.4 (3)	N1—C1—C2	123.4 (3)
C1—N1—C5	118.2 (3)	N1—C1—H1B	118.3
C1—N1—Re	124.3 (2)	C2—C1—H1B	118.3
C5—N1—Re	117.4 (2)	O21—C21—Re	178.1 (3)
C11—N2—C15	118.6 (3)	C12—C13—C14	119.0 (3)
C11—N2—Re	124.2 (2)	C12—C13—H13A	120.5
C15—N2—Re	117.2 (2)	C14—C13—H13A	120.5
O31—C31—Re	179.7 (3)	C51—C52—H52A	109.5
C13—C12—C11	118.7 (3)	C51—C52—H52B	109.5
C13—C12—H12A	120.6	H52A—C52—H52B	109.5
C11—C12—H12A	120.6	C51—C52—H52C	109.5
N2—C11—C12	122.7 (3)	H52A—C52—H52C	109.5
N2—C11—H11A	118.6	H52B—C52—H52C	109.5
C12—C11—H11A	118.6	O1—Cl—O3	109.8 (2)
O41—C41—Re	176.9 (3)	O1—Cl—O4	109.6 (2)
N1—C5—C4	121.0 (3)	O3—Cl—O4	108.90 (18)
N1—C5—C15	115.0 (3)	O1—Cl—O2	109.93 (17)
C4—C5—C15	123.9 (3)	O3—Cl—O2	109.26 (17)
C15—C14—C13	119.7 (3)	O4—Cl—O2	109.32 (16)