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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032246/rz6027sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032246/rz6027Isup2.hkl
Contains datablock I

CCDC reference: 262262

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 top

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 top
Crystal data top
[Re(C2H3N)(C10H8N2)(CO)3]ClO4F(000) = 2160
Mr = 566.92Dx = 2.163 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4993 reflections
a = 33.745 (5) Åθ = 3.3–27.5°
b = 6.3132 (11) ŵ = 7.18 mm1
c = 18.793 (4) ÅT = 293 K
β = 119.572 (10)°Prism, yellow
V = 3482.1 (11) Å30.55 × 0.40 × 0.30 mm
Z = 8
Data collection top
Rigaku Mercury70
diffractometer
3966 independent reflections
Radiation source: Rotating anode3745 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
Detector resolution: 14.6306 pixels mm-1θmax = 27.5°, θmin = 3.4°
CCD profile–fitting scansh = 4329
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 88
Tmin = 0.043, Tmax = 0.113l = 2423
12732 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.061H-atom parameters constrained
S = 1.09 w = 1/[σ2(Fo2) + (0.0365P)2 + 5.548P]
where P = (Fo2 + 2Fc2)/3
3966 reflections(Δ/σ)max = 0.002
244 parametersΔρmax = 2.50 e Å3
0 restraintsΔρmin = 2.45 e Å3
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
xyzUiso*/Ueq
Re0.570648 (4)1.058495 (18)0.204326 (7)0.01148 (6)
N10.63532 (9)0.9050 (4)0.23938 (16)0.0125 (5)
N20.62202 (9)1.2595 (4)0.29842 (15)0.0129 (5)
N30.58441 (9)1.2290 (4)0.12046 (16)0.0159 (5)
C310.51723 (11)1.2289 (5)0.17478 (19)0.0185 (7)
C120.64638 (13)1.5612 (5)0.3874 (2)0.0174 (7)
H12A0.63881.68360.40560.021*
C110.61268 (12)1.4348 (5)0.3279 (2)0.0153 (6)
H11A0.58241.47320.30760.018*
C410.55802 (11)0.9139 (5)0.2809 (2)0.0156 (6)
C50.67384 (11)1.0053 (5)0.29561 (18)0.0144 (6)
C140.70129 (11)1.3182 (5)0.39040 (19)0.0173 (6)
H14A0.73131.27430.41170.021*
C510.58895 (10)1.3152 (5)0.07203 (19)0.0164 (6)
C150.66620 (10)1.2005 (5)0.32970 (18)0.0140 (6)
C20.68122 (12)0.6359 (5)0.2259 (2)0.0194 (7)
H2B0.68280.51030.20160.023*
C30.72039 (12)0.7379 (6)0.2825 (2)0.0211 (7)
H3B0.74890.68260.29680.025*
C40.71649 (12)0.9245 (5)0.3179 (2)0.0181 (7)
H4B0.74250.99490.35640.022*
C10.63979 (11)0.7240 (5)0.20612 (19)0.0169 (6)
H1B0.61350.65500.16780.020*
C210.53262 (12)0.8599 (6)0.1205 (2)0.0214 (7)
C130.69137 (12)1.5016 (6)0.4192 (2)0.0188 (6)
H13A0.71461.58310.45930.023*
C520.59441 (13)1.4297 (6)0.0105 (2)0.0231 (8)
H52A0.61741.53670.03650.028*
H52B0.56601.49520.02740.028*
H52C0.60341.33300.01830.028*
O410.54842 (8)0.8296 (4)0.32447 (14)0.0208 (5)
O40.79882 (11)0.5629 (4)0.4817 (2)0.0329 (7)
O310.48542 (9)1.3297 (4)0.15739 (16)0.0294 (6)
O30.82798 (10)0.5738 (4)0.39152 (18)0.0317 (7)
O20.81000 (9)0.2461 (4)0.42782 (16)0.0258 (5)
O210.51093 (9)0.7376 (5)0.07130 (16)0.0344 (6)
O10.87303 (11)0.4419 (5)0.5246 (2)0.0430 (8)
Cl0.82773 (3)0.45588 (12)0.45672 (5)0.01887 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re0.00864 (8)0.01332 (8)0.01116 (8)0.00090 (4)0.00386 (6)0.00004 (4)
N10.0101 (13)0.0149 (12)0.0124 (12)0.0004 (10)0.0055 (11)0.0009 (10)
N20.0130 (13)0.0145 (12)0.0124 (12)0.0010 (10)0.0072 (10)0.0009 (9)
N30.0138 (13)0.0180 (13)0.0141 (13)0.0005 (10)0.0054 (11)0.0015 (10)
C310.0164 (16)0.0215 (16)0.0161 (15)0.0001 (13)0.0070 (13)0.0032 (12)
C120.0236 (18)0.0161 (16)0.0153 (16)0.0011 (12)0.0117 (14)0.0022 (11)
C110.0153 (16)0.0165 (16)0.0157 (15)0.0006 (11)0.0089 (13)0.0004 (11)
C410.0095 (15)0.0171 (15)0.0175 (15)0.0036 (11)0.0046 (13)0.0003 (12)
C50.0137 (15)0.0161 (14)0.0133 (14)0.0017 (13)0.0067 (12)0.0022 (12)
C140.0141 (15)0.0203 (16)0.0156 (14)0.0015 (12)0.0060 (12)0.0020 (12)
C510.0121 (14)0.0192 (15)0.0141 (14)0.0001 (12)0.0036 (12)0.0031 (12)
C150.0145 (15)0.0156 (15)0.0121 (14)0.0001 (12)0.0067 (12)0.0007 (11)
C20.0262 (18)0.0160 (16)0.0191 (16)0.0051 (13)0.0135 (14)0.0011 (12)
C30.0195 (17)0.0254 (17)0.0207 (16)0.0037 (13)0.0117 (14)0.0020 (13)
C40.0128 (16)0.0217 (17)0.0179 (16)0.0010 (12)0.0061 (13)0.0011 (12)
C10.0197 (16)0.0160 (15)0.0164 (15)0.0009 (12)0.0099 (13)0.0016 (12)
C210.0182 (17)0.0240 (18)0.0212 (17)0.0028 (14)0.0092 (14)0.0000 (14)
C130.0206 (17)0.0202 (15)0.0144 (15)0.0068 (14)0.0076 (13)0.0035 (13)
C520.0228 (19)0.030 (2)0.0172 (17)0.0033 (13)0.0101 (15)0.0030 (13)
O410.0166 (12)0.0257 (13)0.0208 (12)0.0012 (10)0.0097 (10)0.0070 (10)
O40.0345 (17)0.0297 (16)0.0424 (17)0.0048 (11)0.0250 (15)0.0137 (12)
O310.0206 (13)0.0360 (15)0.0303 (14)0.0127 (12)0.0115 (11)0.0115 (12)
O30.0281 (16)0.0344 (16)0.0321 (15)0.0057 (11)0.0145 (13)0.0027 (11)
O20.0238 (13)0.0248 (13)0.0285 (13)0.0064 (10)0.0128 (11)0.0098 (10)
O210.0268 (15)0.0382 (16)0.0298 (14)0.0130 (12)0.0075 (12)0.0164 (12)
O10.0224 (16)0.045 (2)0.0344 (17)0.0021 (12)0.0070 (13)0.0014 (13)
Cl0.0145 (4)0.0203 (4)0.0186 (4)0.0033 (3)0.0057 (3)0.0043 (3)
Geometric parameters (Å, º) top
Re—N12.172 (3)C14—C131.387 (5)
Re—N22.172 (3)C14—H14A0.9300
Re—N32.140 (3)C51—C521.451 (5)
Re—C211.925 (4)C2—C11.374 (5)
Re—C311.931 (3)C2—C31.380 (5)
Re—C411.921 (3)C2—H2B0.9300
N3—C511.133 (4)C3—C41.391 (5)
N1—C11.346 (4)C3—H3B0.9300
N1—C51.361 (4)C4—H4B0.9300
N2—C111.343 (4)C1—H1B0.9300
N2—C151.357 (4)C21—O211.148 (4)
C31—O311.148 (4)C13—H13A0.9300
C12—C131.381 (5)C52—H52A0.9600
C12—C111.387 (5)C52—H52B0.9600
C12—H12A0.9300C52—H52C0.9600
C11—H11A0.9300O4—Cl1.442 (3)
C41—O411.149 (4)O3—Cl1.437 (3)
C5—C41.383 (5)O2—Cl1.444 (3)
C5—C151.469 (4)O1—Cl1.431 (3)
C14—C151.386 (4)
N1—Re—N274.63 (10)C15—C14—H14A120.1
N1—Re—N384.08 (10)C13—C14—H14A120.1
N1—Re—C2197.00 (13)N3—C51—C52178.7 (4)
N1—Re—C31172.62 (12)N2—C15—C14121.3 (3)
N1—Re—C4197.01 (12)N2—C15—C5115.7 (3)
N2—Re—N385.96 (10)C14—C15—C5123.1 (3)
N2—Re—C21171.42 (13)C1—C2—C3118.6 (3)
N2—Re—C3199.51 (12)C1—C2—H2B120.7
N2—Re—C4192.92 (12)C3—C2—H2B120.7
N3—Re—C2191.37 (13)C2—C3—C4118.9 (3)
N3—Re—C3191.09 (12)C2—C3—H3B120.6
N3—Re—C41178.18 (12)C4—C3—H3B120.6
C21—Re—C3188.68 (15)C5—C4—C3119.9 (3)
C21—Re—C4189.94 (14)C5—C4—H4B120.1
C31—Re—C4187.68 (13)C3—C4—H4B120.1
C51—N3—Re175.4 (3)N1—C1—C2123.4 (3)
C1—N1—C5118.2 (3)N1—C1—H1B118.3
C1—N1—Re124.3 (2)C2—C1—H1B118.3
C5—N1—Re117.4 (2)O21—C21—Re178.1 (3)
C11—N2—C15118.6 (3)C12—C13—C14119.0 (3)
C11—N2—Re124.2 (2)C12—C13—H13A120.5
C15—N2—Re117.2 (2)C14—C13—H13A120.5
O31—C31—Re179.7 (3)C51—C52—H52A109.5
C13—C12—C11118.7 (3)C51—C52—H52B109.5
C13—C12—H12A120.6H52A—C52—H52B109.5
C11—C12—H12A120.6C51—C52—H52C109.5
N2—C11—C12122.7 (3)H52A—C52—H52C109.5
N2—C11—H11A118.6H52B—C52—H52C109.5
C12—C11—H11A118.6O1—Cl—O3109.8 (2)
O41—C41—Re176.9 (3)O1—Cl—O4109.6 (2)
N1—C5—C4121.0 (3)O3—Cl—O4108.90 (18)
N1—C5—C15115.0 (3)O1—Cl—O2109.93 (17)
C4—C5—C15123.9 (3)O3—Cl—O2109.26 (17)
C15—C14—C13119.7 (3)O4—Cl—O2109.32 (16)
 

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