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The title compound, (C8H20N)[Re2(C5H4NO)(CH3O)2(CO)6], was obtained from a ligand-substitution reaction of (Et4N)[Re2(OMe)3(CO)6] with 2-hydroxy­pyridine in methanol solvent. Both Re centers are in an approximate octa­hedral geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806034805/ci2152sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806034805/ci2152Isup2.hkl
Contains datablock I

CCDC reference: 624164

Key indicators

  • Single-crystal X-ray study
  • T = 110 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.023
  • wR factor = 0.045
  • Data-to-parameter ratio = 45.6

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 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 0 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2003); cell refinement: APEX2; data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.

Tetraethylammonium di-µ-methoxo-µ-pyridin-2-olato-bis[tricarbonylrhenium(I)] top
Crystal data top
(C8H20N)[Re2(C5H4NO)(CH3O)2(CO)6]F(000) = 1568
Mr = 826.87Dx = 2.131 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9939 reflections
a = 9.3185 (12) Åθ = 2.5–38.3°
b = 25.148 (3) ŵ = 9.43 mm1
c = 11.7267 (14) ÅT = 110 K
β = 110.288 (3)°Block, colorless
V = 2577.5 (5) Å30.22 × 0.19 × 0.12 mm
Z = 4
Data collection top
Bruker X8 APEX area-detector
diffractometer
14267 independent reflections
Radiation source: fine-focus sealed tube12348 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
φ and ω scansθmax = 38.3°, θmin = 2.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1616
Tmin = 0.142, Tmax = 0.319k = 4340
117327 measured reflectionsl = 2017
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.045H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.013P)2 + 2.7693P]
where P = (Fo2 + 2Fc2)/3
14267 reflections(Δ/σ)max = 0.006
313 parametersΔρmax = 1.77 e Å3
0 restraintsΔρmin = 1.16 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
Re10.783967 (7)0.825946 (3)0.751757 (6)0.01156 (2)
Re20.627565 (8)0.932821 (3)0.830866 (6)0.01302 (2)
O10.91605 (18)0.76682 (7)0.99444 (14)0.0263 (3)
O20.6742 (2)0.71706 (6)0.63755 (15)0.0277 (3)
O31.09289 (17)0.79910 (7)0.72609 (15)0.0246 (3)
O40.7044 (2)0.90988 (7)1.10158 (14)0.0287 (3)
O50.30364 (19)0.96516 (8)0.81504 (18)0.0323 (4)
O60.71257 (19)1.04876 (6)0.90300 (15)0.0251 (3)
O70.57699 (14)0.85274 (5)0.76969 (12)0.0143 (2)
O80.83770 (14)0.90410 (5)0.82112 (12)0.0138 (2)
O90.59704 (15)0.94470 (5)0.64342 (12)0.0152 (2)
N10.68863 (16)0.86885 (6)0.57582 (13)0.0119 (2)
N20.16081 (18)0.62510 (7)0.88616 (16)0.0179 (3)
C10.8639 (2)0.79033 (7)0.90396 (17)0.0167 (3)
C20.7143 (2)0.75838 (7)0.68002 (17)0.0167 (3)
C30.9756 (2)0.81008 (8)0.73321 (17)0.0168 (3)
C40.6721 (2)0.91883 (8)0.99878 (18)0.0195 (3)
C50.4251 (2)0.95271 (8)0.82077 (19)0.0205 (3)
C60.6828 (2)1.00475 (8)0.87541 (17)0.0170 (3)
C70.4964 (3)0.81917 (9)0.8261 (2)0.0243 (4)
H7A0.55830.81420.91200.036*
H7B0.47700.78460.78510.036*
H7C0.39880.83580.81970.036*
C80.9795 (2)0.91489 (8)0.91429 (19)0.0207 (4)
H8A1.06360.90400.88730.031*
H8B0.98550.89500.98770.031*
H8C0.98740.95310.93220.031*
C90.63005 (19)0.91943 (7)0.56025 (16)0.0120 (3)
C100.6969 (2)0.84289 (7)0.47584 (16)0.0143 (3)
H100.73190.80710.48600.017*
C110.6584 (2)0.86466 (8)0.36226 (17)0.0161 (3)
H110.66200.84420.29520.019*
C120.6133 (2)0.91836 (8)0.34830 (16)0.0158 (3)
H120.59190.93570.27220.019*
C130.6006 (2)0.94522 (7)0.44582 (16)0.0143 (3)
H130.57180.98160.43730.017*
C140.3055 (2)0.65062 (9)0.97293 (19)0.0217 (4)
H14A0.34100.62961.04890.026*
H14B0.38610.64880.93600.026*
C150.2875 (3)0.70823 (10)1.0050 (2)0.0284 (4)
H15A0.21080.71051.04450.043*
H15B0.25450.72970.93060.043*
H15C0.38570.72161.06030.043*
C160.0990 (2)0.65714 (9)0.7692 (2)0.0241 (4)
H16A0.01200.63740.71140.029*
H16B0.05860.69120.78760.029*
C170.2136 (3)0.66913 (9)0.7071 (2)0.0276 (4)
H17A0.25810.63580.69150.041*
H17B0.29490.69200.75970.041*
H17C0.16170.68740.62990.041*
C180.0355 (2)0.62333 (9)0.9407 (2)0.0263 (4)
H18A0.01360.66010.95970.032*
H18B0.05850.60920.87880.032*
C190.0713 (3)0.59017 (11)1.0545 (3)0.0360 (6)
H19A0.09400.55361.03730.054*
H19B0.01710.59021.08160.054*
H19C0.16020.60521.11850.054*
C200.2049 (2)0.56906 (8)0.8609 (2)0.0208 (4)
H20A0.28000.57190.81880.025*
H20B0.25660.55120.93980.025*
C210.0743 (3)0.53396 (9)0.7854 (2)0.0285 (4)
H21A0.11500.49980.77040.043*
H21B0.01990.55140.70770.043*
H21C0.00340.52800.82940.043*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.01298 (3)0.00995 (3)0.01114 (3)0.00028 (2)0.00342 (2)0.00104 (2)
Re20.01627 (3)0.01243 (3)0.01075 (3)0.00055 (2)0.00518 (2)0.00074 (2)
O10.0262 (7)0.0260 (8)0.0206 (7)0.0047 (6)0.0006 (6)0.0100 (6)
O20.0448 (9)0.0157 (7)0.0222 (7)0.0068 (6)0.0112 (7)0.0029 (6)
O30.0195 (6)0.0262 (8)0.0294 (8)0.0041 (6)0.0100 (6)0.0007 (6)
O40.0460 (10)0.0252 (8)0.0162 (7)0.0004 (7)0.0126 (7)0.0008 (6)
O50.0251 (8)0.0364 (10)0.0401 (10)0.0064 (7)0.0170 (7)0.0024 (8)
O60.0318 (8)0.0169 (7)0.0230 (7)0.0020 (6)0.0051 (6)0.0029 (6)
O70.0144 (5)0.0138 (5)0.0153 (6)0.0019 (4)0.0059 (4)0.0004 (4)
O80.0125 (5)0.0137 (5)0.0131 (5)0.0006 (4)0.0018 (4)0.0006 (4)
O90.0199 (6)0.0141 (5)0.0120 (5)0.0048 (5)0.0059 (4)0.0001 (4)
N10.0124 (6)0.0111 (6)0.0118 (6)0.0010 (5)0.0038 (5)0.0004 (5)
N20.0131 (6)0.0171 (7)0.0221 (8)0.0028 (5)0.0044 (5)0.0008 (6)
C10.0170 (7)0.0149 (7)0.0169 (8)0.0031 (6)0.0042 (6)0.0015 (6)
C20.0213 (8)0.0140 (7)0.0143 (7)0.0002 (6)0.0056 (6)0.0030 (6)
C30.0179 (7)0.0157 (7)0.0160 (7)0.0001 (6)0.0050 (6)0.0010 (6)
C40.0275 (9)0.0164 (8)0.0159 (8)0.0003 (7)0.0093 (7)0.0012 (6)
C50.0233 (8)0.0201 (9)0.0199 (9)0.0007 (7)0.0098 (7)0.0028 (7)
C60.0199 (8)0.0176 (8)0.0125 (7)0.0011 (6)0.0044 (6)0.0001 (6)
C70.0259 (9)0.0247 (10)0.0243 (10)0.0055 (8)0.0114 (8)0.0005 (8)
C80.0195 (8)0.0187 (8)0.0182 (8)0.0022 (7)0.0006 (6)0.0017 (7)
C90.0122 (6)0.0109 (6)0.0124 (7)0.0008 (5)0.0036 (5)0.0002 (5)
C100.0150 (7)0.0141 (7)0.0138 (7)0.0024 (6)0.0048 (6)0.0008 (6)
C110.0179 (7)0.0180 (8)0.0125 (7)0.0023 (6)0.0054 (6)0.0014 (6)
C120.0177 (7)0.0184 (8)0.0119 (7)0.0033 (6)0.0057 (6)0.0012 (6)
C130.0170 (7)0.0132 (7)0.0131 (7)0.0021 (6)0.0057 (6)0.0015 (6)
C140.0145 (7)0.0266 (10)0.0207 (9)0.0017 (7)0.0020 (6)0.0013 (7)
C150.0267 (10)0.0280 (11)0.0286 (11)0.0036 (8)0.0074 (8)0.0061 (9)
C160.0202 (8)0.0184 (9)0.0253 (10)0.0038 (7)0.0027 (7)0.0032 (7)
C170.0346 (11)0.0223 (10)0.0221 (10)0.0011 (8)0.0051 (8)0.0042 (8)
C180.0202 (9)0.0228 (10)0.0395 (13)0.0023 (7)0.0149 (9)0.0025 (9)
C190.0444 (14)0.0304 (12)0.0462 (15)0.0050 (11)0.0320 (13)0.0027 (11)
C200.0191 (8)0.0182 (8)0.0246 (9)0.0058 (7)0.0070 (7)0.0028 (7)
C210.0286 (10)0.0206 (10)0.0365 (12)0.0000 (8)0.0116 (9)0.0030 (9)
Geometric parameters (Å, º) top
Re1—C11.9028 (19)C9—C131.429 (2)
Re1—C21.9073 (19)C10—C111.368 (3)
Re1—C31.9141 (19)C10—H100.95
Re1—O82.1195 (13)C11—C121.407 (3)
Re1—O72.1212 (13)C11—H110.95
Re1—N12.2223 (15)C12—C131.368 (3)
Re2—C41.899 (2)C12—H120.95
Re2—C61.904 (2)C13—H130.95
Re2—C51.915 (2)C14—C151.520 (3)
Re2—O82.1271 (13)C14—H14A0.99
Re2—O72.1350 (13)C14—H14B0.99
Re2—O92.1374 (13)C15—H15A0.98
O1—C11.164 (2)C15—H15B0.98
O2—C21.157 (2)C15—H15C0.98
O3—C31.158 (2)C16—C171.517 (3)
O4—C41.159 (2)C16—H16A0.99
O5—C51.154 (3)C16—H16B0.99
O6—C61.159 (2)C17—H17A0.98
O7—C71.435 (2)C17—H17B0.98
O8—C81.418 (2)C17—H17C0.98
O9—C91.287 (2)C18—C191.510 (4)
N1—C101.367 (2)C18—H18A0.99
N1—C91.371 (2)C18—H18B0.99
N2—C181.514 (3)C19—H19A0.98
N2—C141.521 (3)C19—H19B0.98
N2—C161.521 (3)C19—H19C0.98
N2—C201.525 (3)C20—C211.515 (3)
C7—H7A0.98C20—H20A0.99
C7—H7B0.98C20—H20B0.99
C7—H7C0.98C21—H21A0.98
C8—H8A0.98C21—H21B0.98
C8—H8B0.98C21—H21C0.98
C8—H8C0.98
C1—Re1—C287.54 (8)O9—C9—N1123.06 (16)
C1—Re1—C386.07 (8)O9—C9—C13117.97 (15)
C2—Re1—C387.28 (8)N1—C9—C13118.95 (15)
C1—Re1—O896.49 (7)N1—C10—C11124.76 (17)
C2—Re1—O8173.89 (7)N1—C10—H10117.6
C3—Re1—O897.55 (7)C11—C10—H10117.6
C1—Re1—O797.47 (7)C10—C11—C12117.67 (17)
C2—Re1—O798.30 (7)C10—C11—H11121.2
C3—Re1—O7173.49 (7)C12—C11—H11121.2
O8—Re1—O776.67 (5)C13—C12—C11119.05 (17)
C1—Re1—N1178.80 (7)C13—C12—H12120.5
C2—Re1—N193.30 (7)C11—C12—H12120.5
C3—Re1—N194.83 (7)C12—C13—C9121.12 (17)
O8—Re1—N182.61 (5)C12—C13—H13119.4
O7—Re1—N181.57 (5)C9—C13—H13119.4
C4—Re2—C687.16 (8)C15—C14—N2114.80 (17)
C4—Re2—C588.21 (9)C15—C14—H14A108.6
C6—Re2—C586.31 (9)N2—C14—H14A108.6
C4—Re2—O896.81 (7)C15—C14—H14B108.6
C6—Re2—O899.85 (7)N2—C14—H14B108.6
C5—Re2—O8172.20 (7)H14A—C14—H14B107.5
C4—Re2—O796.72 (7)C14—C15—H15A109.5
C6—Re2—O7174.74 (7)C14—C15—H15B109.5
C5—Re2—O797.34 (7)H15A—C15—H15B109.5
O8—Re2—O776.21 (5)C14—C15—H15C109.5
C4—Re2—O9174.59 (7)H15A—C15—H15C109.5
C6—Re2—O994.37 (7)H15B—C15—H15C109.5
C5—Re2—O997.06 (7)C17—C16—N2115.38 (17)
O8—Re2—O977.81 (5)C17—C16—H16A108.4
O7—Re2—O981.44 (5)N2—C16—H16A108.4
C7—O7—Re1119.88 (12)C17—C16—H16B108.4
C7—O7—Re2119.34 (12)N2—C16—H16B108.4
Re1—O7—Re2103.33 (5)H16A—C16—H16B107.5
C8—O8—Re1120.40 (11)C16—C17—H17A109.5
C8—O8—Re2121.51 (12)C16—C17—H17B109.5
Re1—O8—Re2103.66 (5)H17A—C17—H17B109.5
C9—O9—Re2136.76 (12)C16—C17—H17C109.5
C10—N1—C9117.83 (15)H17A—C17—H17C109.5
C10—N1—Re1116.17 (11)H17B—C17—H17C109.5
C9—N1—Re1125.91 (11)C19—C18—N2115.06 (18)
C18—N2—C14111.36 (17)C19—C18—H18A108.5
C18—N2—C16106.86 (16)N2—C18—H18A108.5
C14—N2—C16110.51 (16)C19—C18—H18B108.5
C18—N2—C20110.71 (16)N2—C18—H18B108.5
C14—N2—C20106.50 (15)H18A—C18—H18B107.5
C16—N2—C20110.96 (17)C18—C19—H19A109.5
O1—C1—Re1176.72 (19)C18—C19—H19B109.5
O2—C2—Re1178.92 (19)H19A—C19—H19B109.5
O3—C3—Re1177.18 (18)C18—C19—H19C109.5
O4—C4—Re2177.6 (2)H19A—C19—H19C109.5
O5—C5—Re2179.4 (2)H19B—C19—H19C109.5
O6—C6—Re2178.08 (18)C21—C20—N2115.84 (17)
O7—C7—H7A109.5C21—C20—H20A108.3
O7—C7—H7B109.5N2—C20—H20A108.3
H7A—C7—H7B109.5C21—C20—H20B108.3
O7—C7—H7C109.5N2—C20—H20B108.3
H7A—C7—H7C109.5H20A—C20—H20B107.4
H7B—C7—H7C109.5C20—C21—H21A109.5
O8—C8—H8A109.5C20—C21—H21B109.5
O8—C8—H8B109.5H21A—C21—H21B109.5
H8A—C8—H8B109.5C20—C21—H21C109.5
O8—C8—H8C109.5H21A—C21—H21C109.5
H8A—C8—H8C109.5H21B—C21—H21C109.5
H8B—C8—H8C109.5
 

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