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In the title compound [ReCl(C34H38N4)(CO)3], the Re atom has a distorted octahedral configuration. The bi­pyridine part of the DEAS–bpy ligand and two carbonyl groups occupy the equatorial plane of the complex, with the third carbonyl ligand and the Cl atom in the axial positions. The organic ligand is essentially planar, giving rise to an extended π-conjugated system.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801004573/cf6052sup1.cif
Contains datablocks reco3cl, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801004573/cf6052Isup2.hkl
Contains datablock I

CCDC reference: 162804

Key indicators

  • Single-crystal X-ray study
  • T = 90 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.028
  • wR factor = 0.065
  • Data-to-parameter ratio = 25.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry
Red Alert Alert Level A:
ABSTM_02 Alert A Test not performed as the _exptl_absorpt_correction_type has not been identified. See test ABSTY_01. ABSTY_01 Alert A The absorption correction should be one of the following * none * analytical * integration * numerical * gaussian * empirical * psi-scan * multi-scan * refdelf * sphere * cylinder
Amber Alert Alert Level B:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 32.51 From the CIF: _reflns_number_total 10508 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 11793 Completeness (_total/calc) 89.10% Alert B: < 90% complete (theta max?)
Yellow Alert Alert Level C:
PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 3 C3 -RE1 -N1 -C8 -134.10 0.50 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 8 C3 -RE1 -N1 -C4 37.80 0.60 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 12 C1 -RE1 -N2 -C25 -175.20 0.70 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 17 C1 -RE1 -N2 -C21 1.80 0.80 1.555 1.555 1.555 1.555
2 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
4 Alert Level C = Please check

Comment top

ReI–polypyridine–carbonyl complexes have interesting photophysical properties (Ziessel et al., 1998); they can be used in photo- and electro-reduction reactions (Hawecker et al., 1986; O'Toole et al., 1985; Kutal et al., 1987). It has also been suggested that they may form new materials possessing non-linear optical properties (Lehn, 1987). Therefore, knowledge of the molecular and crystal structure of such complexes is essential for understanding and explaining their properties. In the present communication, we report results of an X-ray structure investigation of the title complex, (I).

The Re atom in (I) has a distorted octahedral configuration, with the bipyridine moiety of the organic ligand and two carbonyl groups in the equatorial plane, and one carbonyl ligand and a Cl atom in the axial positions (Fig. 1). The bond angle N1—Re1—N2 of 74.55 (8)° is far away from the ideal octahedral value. However, the C1—Re1—C3 angle is almost 89.4 (1)°. The axial CO ligand is displaced out of the DEAS–bpy plane [C2—Re1—N1 is 99.01 (9)°], while Cl1 is displaced towards the organic part of the molecule [N1—Re1—Cl1 is 82.94 (6)°]. Moreover, the C3 atom is considerably displaced by 0.21 Å from a plane through the other equatorial atoms. Despite the significant distortion of the Re atom configuration from octahedral, all Re—C and C—O distances are similar (Table 1), though the axial Re—C bond is somewhat shorter than the equatorial bonds. The C—O bond lengths indicate significant π-back donation from the Re atom. This can be explained by strong electron-donating properties of the organic ligand.

DEAS-bpy contains two identical parts, each consisting of the diethylaminophenyl and pyridine groups connected by an ethylene moiety. The two parts are slightly twisted with respect to each other, the dihedral angle between them being 3°. Each half of DEAS–bpy is distorted from planarity. The relevant torsion angles C23—C26—C27—C28, C24—C23—C26—C27, C26—C27—C28—C29, C6—C9—C10—C11, C5—C6—C9—C10, C9—C10—C11—C16 are 177.5 (2), -173.6 (3), -171.7 (3), 174.9 (2), -173.8 (3), and 173.4 (3)°, respectively. This non-planarity is sufficiently small to conserve the extended π-conjugated system of the organic ligand. Accordingly, the amine N3 and N4 atoms are almost coplanar with the C atoms to which they are bonded [the sums of the bond angles are 360.0 (6) and 357.6 (6)°, respectively]. Both methyl groups of each diethylamino substituent are displaced in opposite directions with respect to the mean DEAS–bpy plane.

In the crystal, molecules of (I) form dimers along the crystallographic c axis; the shortest contact in a dimer is Cl1···H5A(1 - x, 1 - y, -z) 2.65 Å.

Experimental top

Compound (I) was synthesized as described in the literature (Juris et al., 1988). Crystals appropriate for X-ray structure analysis were grown by diffusion of ether into a solution of compound (I) in dichloromethane.

Refinement top

The positions of all H atoms were found from difference Fourier syntheses. Methyl groups were refined with torsional freedom, other H atoms with a riding model. U(H) was set at 1.2 (1.5 for methyl groups) times Ueq(C). The largest positive and negative features of the final difference synthesis lie within 0.9 Å of the Re atom.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SHELXTL (Sheldrick, 1997); 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.

Figures top
[Figure 1] Fig. 1. A view of (I) with displacement ellipsoids drawn at the 50% probability level. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. A view of the dimer as found in the crystal. H atoms have been omitted for clarity.
{4,4'-Bis[p-(diethylamino)-alfa-styryl]-2,2' -bipyridine}chlorotricarbonylrhenium(I) top
Crystal data top
[ReCl(C34H38N4)(CO)3]Dx = 1.650 Mg m3
Mr = 808.36Melting point: not measured K
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 14.4908 (5) ÅCell parameters from 846 reflections
b = 23.1755 (5) Åθ = 2–30°
c = 9.6971 (5) ŵ = 3.86 mm1
β = 91.899 (2)°T = 90 K
V = 3254.8 (2) Å3Plate, red
Z = 40.3 × 0.2 × 0.1 mm
F(000) = 1616
Data collection top
CCD area-detector
diffractometer
10508 independent reflections
Radiation source: rotating anode8209 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
ϕ and ω scansθmax = 32.5°, θmin = 1.4°
Absorption correction: (SADABS; bruker, 1998)
?
h = 2121
Tmin = 0.391, Tmax = 0.699k = 2934
36470 measured reflectionsl = 1413
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.028H-atom parameters constrained
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0323P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max = 0.006
10508 reflectionsΔρmax = 1.75 e Å3
420 parametersΔρmin = 1.72 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00096 (8)
Crystal data top
[ReCl(C34H38N4)(CO)3]V = 3254.8 (2) Å3
Mr = 808.36Z = 4
Monoclinic, P21/cMo Kα radiation
a = 14.4908 (5) ŵ = 3.86 mm1
b = 23.1755 (5) ÅT = 90 K
c = 9.6971 (5) Å0.3 × 0.2 × 0.1 mm
β = 91.899 (2)°
Data collection top
CCD area-detector
diffractometer
10508 independent reflections
Absorption correction: (SADABS; bruker, 1998)
?
8209 reflections with I > 2σ(I)
Tmin = 0.391, Tmax = 0.699Rint = 0.058
36470 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.065H-atom parameters constrained
S = 0.97Δρmax = 1.75 e Å3
10508 reflectionsΔρmin = 1.72 e Å3
420 parameters
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Re10.215386 (6)0.489912 (4)0.066402 (10)0.01544 (4)
Cl10.33247 (4)0.45493 (3)0.24092 (6)0.02012 (12)
O10.10862 (14)0.55550 (9)0.2851 (2)0.0315 (5)
O20.06605 (13)0.52626 (9)0.1454 (2)0.0286 (4)
O30.09783 (12)0.38165 (9)0.1093 (2)0.0258 (4)
N10.31880 (13)0.55588 (9)0.0316 (2)0.0166 (4)
N20.30262 (12)0.45487 (9)0.0917 (2)0.0147 (4)
N30.89867 (14)0.84891 (10)0.0419 (2)0.0217 (5)
N40.79002 (14)0.31395 (10)0.8427 (2)0.0216 (5)
C10.14821 (17)0.52952 (12)0.2043 (3)0.0209 (5)
C20.12411 (16)0.51392 (11)0.0665 (3)0.0207 (5)
C30.14085 (15)0.42258 (12)0.0944 (3)0.0184 (5)
C40.38481 (15)0.54384 (11)0.0610 (2)0.0154 (5)
C50.45826 (16)0.58008 (11)0.0814 (3)0.0183 (5)
H5A0.50210.57030.14840.022*
C60.46953 (17)0.63075 (11)0.0059 (3)0.0193 (5)
C70.40197 (17)0.64244 (11)0.0904 (3)0.0214 (5)
H7A0.40620.67630.14560.026*
C80.32929 (17)0.60458 (12)0.1048 (3)0.0209 (5)
H8A0.28420.61360.17040.025*
C90.55102 (17)0.66668 (12)0.0313 (3)0.0217 (5)
H9A0.58850.65520.10500.026*
C100.57749 (17)0.71350 (12)0.0384 (3)0.0220 (5)
H10A0.53750.72700.10710.026*
C110.66233 (16)0.74634 (12)0.0194 (3)0.0213 (5)
C120.73239 (17)0.72844 (12)0.0680 (3)0.0220 (5)
H12A0.72590.69260.11470.026*
C130.81064 (17)0.76139 (12)0.0882 (3)0.0219 (5)
H13A0.85630.74780.14840.026*
C140.82320 (16)0.81477 (11)0.0207 (3)0.0186 (5)
C150.75400 (17)0.83178 (12)0.0707 (3)0.0211 (5)
H15A0.76050.86710.11980.025*
C160.67758 (17)0.79797 (12)0.0893 (3)0.0215 (5)
H16A0.63320.81040.15270.026*
C170.97011 (17)0.83081 (13)0.1354 (3)0.0241 (6)
H17A0.98150.78900.12210.029*
H17B1.02810.85130.10970.029*
C180.94727 (19)0.84179 (14)0.2881 (3)0.0296 (6)
H18A1.00230.83490.34180.044*
H18B0.92710.88190.30070.044*
H18C0.89770.81570.31970.044*
C190.90892 (18)0.90586 (12)0.0221 (3)0.0263 (6)
H19A0.97530.91600.02770.032*
H19B0.88690.90380.11750.032*
C200.8571 (2)0.95339 (14)0.0537 (3)0.0367 (7)
H20A0.87120.99050.00940.055*
H20B0.79060.94600.05110.055*
H20C0.87590.95450.14980.055*
C210.37290 (15)0.48832 (11)0.1345 (3)0.0151 (4)
C220.43071 (15)0.47071 (11)0.2385 (3)0.0174 (5)
H22A0.47950.49510.26560.021*
C230.41739 (15)0.41755 (11)0.3029 (3)0.0172 (5)
C240.34359 (16)0.38404 (12)0.2582 (3)0.0186 (5)
H24A0.33080.34770.30000.022*
C250.28946 (15)0.40378 (11)0.1536 (3)0.0174 (5)
H25A0.24050.38000.12420.021*
C260.47621 (16)0.39445 (12)0.4085 (3)0.0203 (5)
H26A0.45750.35890.44930.024*
C270.55387 (16)0.41793 (11)0.4544 (3)0.0180 (5)
H27A0.57220.45430.41750.022*
C280.61233 (15)0.39184 (11)0.5570 (3)0.0173 (5)
C290.69850 (16)0.41584 (11)0.5858 (3)0.0198 (5)
H29A0.71690.45070.54110.024*
C300.75763 (17)0.39031 (12)0.6774 (3)0.0209 (5)
H30A0.81590.40760.69280.025*
C310.73285 (16)0.33942 (11)0.7478 (3)0.0191 (5)
C320.64613 (16)0.31511 (12)0.7202 (3)0.0197 (5)
H32A0.62690.28070.76610.024*
C330.58881 (16)0.34088 (11)0.6268 (3)0.0198 (5)
H33A0.53120.32320.60940.024*
C340.76058 (19)0.26263 (13)0.9191 (3)0.0244 (6)
H34A0.79580.26041.00470.029*
H34B0.69450.26690.94640.029*
C350.77303 (18)0.20632 (12)0.8410 (3)0.0251 (6)
H35A0.74850.17450.89770.038*
H35B0.73980.20820.75470.038*
H35C0.83890.19980.82020.038*
C360.88844 (18)0.32694 (13)0.8383 (3)0.0269 (6)
H36A0.89670.36920.84720.032*
H36B0.91710.30850.91830.032*
C370.93833 (18)0.30672 (14)0.7073 (3)0.0291 (6)
H37A1.00400.31630.71130.044*
H37B0.93130.26490.69820.044*
H37C0.91200.32590.62760.044*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Re10.01416 (5)0.01235 (6)0.02007 (6)0.00031 (3)0.00446 (3)0.00081 (4)
Cl10.0184 (2)0.0192 (3)0.0228 (3)0.0010 (2)0.0022 (2)0.0026 (2)
O10.0346 (10)0.0269 (12)0.0337 (12)0.0069 (9)0.0137 (9)0.0057 (9)
O20.0209 (8)0.0270 (11)0.0379 (12)0.0023 (8)0.0002 (8)0.0044 (9)
O30.0261 (9)0.0206 (11)0.0311 (11)0.0063 (8)0.0086 (8)0.0018 (8)
N10.0185 (9)0.0118 (11)0.0194 (11)0.0001 (7)0.0013 (8)0.0002 (8)
N20.0144 (8)0.0109 (11)0.0190 (10)0.0003 (7)0.0008 (7)0.0024 (8)
N30.0192 (9)0.0182 (12)0.0280 (12)0.0026 (8)0.0042 (8)0.0018 (9)
N40.0230 (10)0.0171 (12)0.0251 (12)0.0019 (8)0.0063 (9)0.0007 (9)
C10.0221 (10)0.0153 (12)0.0257 (13)0.0017 (10)0.0049 (9)0.0043 (11)
C20.0171 (10)0.0143 (13)0.0311 (14)0.0010 (9)0.0055 (9)0.0022 (11)
C30.0143 (9)0.0220 (14)0.0191 (12)0.0013 (9)0.0042 (8)0.0032 (10)
C40.0162 (9)0.0141 (13)0.0161 (11)0.0021 (8)0.0003 (8)0.0030 (9)
C50.0180 (10)0.0163 (13)0.0207 (13)0.0003 (9)0.0003 (9)0.0027 (10)
C60.0197 (10)0.0157 (13)0.0222 (13)0.0014 (9)0.0046 (9)0.0045 (10)
C70.0276 (12)0.0131 (13)0.0234 (14)0.0006 (10)0.0005 (10)0.0001 (10)
C80.0221 (11)0.0175 (14)0.0233 (14)0.0022 (9)0.0037 (10)0.0012 (10)
C90.0215 (11)0.0193 (14)0.0245 (14)0.0010 (10)0.0015 (10)0.0008 (10)
C100.0212 (11)0.0199 (14)0.0251 (14)0.0028 (9)0.0018 (10)0.0026 (10)
C110.0186 (10)0.0232 (15)0.0220 (13)0.0003 (9)0.0010 (9)0.0070 (10)
C120.0270 (12)0.0155 (14)0.0234 (14)0.0012 (10)0.0029 (10)0.0002 (10)
C130.0227 (11)0.0175 (14)0.0258 (14)0.0015 (10)0.0036 (10)0.0006 (10)
C140.0174 (10)0.0170 (13)0.0213 (13)0.0002 (9)0.0001 (9)0.0016 (10)
C150.0231 (11)0.0189 (14)0.0213 (13)0.0007 (10)0.0015 (9)0.0011 (10)
C160.0210 (11)0.0231 (15)0.0204 (13)0.0029 (10)0.0020 (9)0.0022 (10)
C170.0211 (11)0.0236 (15)0.0277 (15)0.0009 (10)0.0037 (10)0.0021 (11)
C180.0278 (13)0.0344 (18)0.0268 (15)0.0055 (12)0.0033 (11)0.0010 (12)
C190.0280 (13)0.0195 (15)0.0313 (15)0.0048 (11)0.0002 (11)0.0012 (11)
C200.0554 (19)0.0207 (17)0.0335 (17)0.0014 (14)0.0057 (15)0.0021 (13)
C210.0139 (9)0.0150 (12)0.0165 (12)0.0008 (8)0.0000 (8)0.0012 (9)
C220.0160 (9)0.0151 (12)0.0214 (12)0.0004 (9)0.0025 (9)0.0016 (10)
C230.0158 (10)0.0183 (13)0.0175 (12)0.0021 (9)0.0012 (8)0.0003 (9)
C240.0195 (10)0.0145 (13)0.0219 (13)0.0012 (9)0.0001 (9)0.0004 (10)
C250.0164 (10)0.0153 (13)0.0206 (12)0.0010 (9)0.0012 (9)0.0002 (9)
C260.0201 (11)0.0195 (14)0.0215 (13)0.0005 (9)0.0017 (9)0.0046 (10)
C270.0205 (10)0.0143 (13)0.0191 (12)0.0010 (9)0.0005 (9)0.0023 (9)
C280.0182 (10)0.0150 (13)0.0186 (12)0.0022 (9)0.0014 (9)0.0026 (9)
C290.0232 (11)0.0137 (13)0.0225 (13)0.0007 (9)0.0033 (9)0.0004 (10)
C300.0210 (11)0.0165 (14)0.0254 (14)0.0023 (9)0.0067 (10)0.0033 (10)
C310.0218 (11)0.0168 (14)0.0190 (12)0.0039 (9)0.0038 (9)0.0033 (10)
C320.0205 (11)0.0168 (14)0.0217 (13)0.0015 (9)0.0004 (9)0.0001 (10)
C330.0159 (10)0.0190 (14)0.0246 (13)0.0007 (9)0.0010 (9)0.0013 (10)
C340.0304 (13)0.0263 (16)0.0168 (13)0.0043 (11)0.0025 (10)0.0030 (11)
C350.0259 (12)0.0203 (15)0.0292 (15)0.0014 (10)0.0006 (11)0.0019 (11)
C360.0284 (13)0.0202 (15)0.0328 (16)0.0009 (11)0.0131 (11)0.0005 (11)
C370.0241 (12)0.0294 (17)0.0337 (16)0.0025 (11)0.0012 (11)0.0045 (12)
Geometric parameters (Å, º) top
Re1—C21.899 (3)C9—C101.328 (4)
Re1—C11.914 (3)C10—C111.463 (3)
Re1—C31.922 (3)C11—C161.389 (4)
Re1—N12.175 (2)C11—C121.406 (4)
Re1—N22.176 (2)C12—C131.387 (4)
Re1—Cl12.4919 (6)C13—C141.409 (4)
O1—C11.156 (3)C14—C151.416 (3)
O2—C21.155 (3)C15—C161.373 (4)
O3—C31.147 (3)C17—C181.528 (4)
N1—C81.340 (3)C19—C201.510 (4)
N1—C41.362 (3)C21—C221.393 (3)
N2—C251.338 (3)C22—C231.392 (4)
N2—C211.356 (3)C23—C241.402 (3)
N3—C141.371 (3)C23—C261.456 (3)
N3—C171.460 (3)C24—C251.381 (3)
N3—C191.464 (4)C26—C271.339 (3)
N4—C311.390 (3)C27—C281.459 (3)
N4—C361.457 (3)C28—C331.398 (4)
N4—C341.457 (4)C28—C291.403 (3)
C4—C51.375 (3)C29—C301.387 (3)
C4—C211.478 (4)C30—C311.403 (4)
C5—C61.391 (4)C31—C321.411 (3)
C6—C71.402 (4)C32—C331.384 (3)
C6—C91.472 (4)C34—C351.517 (4)
C7—C81.381 (4)C36—C371.515 (4)
C2—Re1—C188.54 (11)N1—C8—C7123.7 (2)
C2—Re1—C387.22 (11)C10—C9—C6126.7 (3)
C1—Re1—C389.41 (11)C9—C10—C11126.2 (3)
C2—Re1—N199.01 (9)C16—C11—C12116.2 (2)
C1—Re1—N198.07 (10)C16—C11—C10120.5 (2)
C3—Re1—N1170.35 (9)C12—C11—C10123.3 (3)
C2—Re1—N292.24 (9)C13—C12—C11122.2 (3)
C1—Re1—N2172.61 (10)C12—C13—C14120.8 (2)
C3—Re1—N297.97 (9)N3—C14—C13121.9 (2)
N1—Re1—N274.55 (8)N3—C14—C15121.2 (2)
C2—Re1—Cl1177.94 (8)C13—C14—C15116.9 (2)
C1—Re1—Cl191.85 (8)C16—C15—C14120.9 (3)
C3—Re1—Cl190.76 (8)C15—C16—C11122.9 (2)
N1—Re1—Cl182.94 (6)N3—C17—C18114.7 (2)
N2—Re1—Cl187.63 (5)N3—C19—C20114.2 (2)
C8—N1—C4116.9 (2)N2—C21—C22122.0 (2)
C8—N1—Re1125.21 (16)N2—C21—C4115.3 (2)
C4—N1—Re1117.44 (16)C22—C21—C4122.7 (2)
C25—N2—C21117.7 (2)C23—C22—C21120.4 (2)
C25—N2—Re1124.67 (15)C22—C23—C24116.6 (2)
C21—N2—Re1117.52 (16)C22—C23—C26124.4 (2)
C14—N3—C17120.9 (2)C24—C23—C26119.0 (2)
C14—N3—C19121.8 (2)C25—C24—C23120.1 (2)
C17—N3—C19117.3 (2)N2—C25—C24123.2 (2)
C31—N4—C36119.8 (2)C27—C26—C23127.0 (2)
C31—N4—C34120.8 (2)C26—C27—C28124.9 (2)
C36—N4—C34117.0 (2)C33—C28—C29116.3 (2)
O1—C1—Re1177.3 (2)C33—C28—C27122.9 (2)
O2—C2—Re1176.7 (2)C29—C28—C27120.8 (2)
O3—C3—Re1178.4 (2)C30—C29—C28122.1 (2)
N1—C4—C5122.3 (2)C29—C30—C31121.1 (2)
N1—C4—C21115.0 (2)N4—C31—C30122.0 (2)
C5—C4—C21122.7 (2)N4—C31—C32120.7 (2)
C4—C5—C6121.2 (2)C30—C31—C32117.3 (2)
C5—C6—C7116.2 (2)C33—C32—C31120.6 (2)
C5—C6—C9118.1 (2)C32—C33—C28122.6 (2)
C7—C6—C9125.7 (2)N4—C34—C35114.9 (2)
C8—C7—C6119.7 (2)N4—C36—C37113.6 (2)
C2—Re1—N1—C896.2 (2)C13—C14—C15—C161.4 (4)
C1—Re1—N1—C86.4 (2)C14—C15—C16—C111.2 (4)
C3—Re1—N1—C8134.1 (5)C12—C11—C16—C153.1 (4)
N2—Re1—N1—C8174.0 (2)C10—C11—C16—C15177.0 (2)
Cl1—Re1—N1—C884.5 (2)C14—N3—C17—C1881.1 (3)
C2—Re1—N1—C491.92 (18)C19—N3—C17—C1896.0 (3)
C1—Re1—N1—C4178.29 (18)C14—N3—C19—C2082.0 (3)
C3—Re1—N1—C437.8 (6)C17—N3—C19—C2095.0 (3)
N2—Re1—N1—C42.08 (17)C25—N2—C21—C220.5 (3)
Cl1—Re1—N1—C487.41 (17)Re1—N2—C21—C22177.77 (18)
C2—Re1—N2—C2579.3 (2)C25—N2—C21—C4179.2 (2)
C1—Re1—N2—C25175.2 (7)Re1—N2—C21—C43.6 (3)
C3—Re1—N2—C258.2 (2)N1—C4—C21—N25.3 (3)
N1—Re1—N2—C25178.0 (2)C5—C4—C21—N2173.1 (2)
Cl1—Re1—N2—C2598.68 (19)N1—C4—C21—C22176.1 (2)
C2—Re1—N2—C2197.77 (18)C5—C4—C21—C225.6 (4)
C1—Re1—N2—C211.8 (8)N2—C21—C22—C230.4 (4)
C3—Re1—N2—C21174.72 (18)C4—C21—C22—C23178.9 (2)
N1—Re1—N2—C210.96 (16)C21—C22—C23—C240.4 (4)
Cl1—Re1—N2—C2184.28 (16)C21—C22—C23—C26177.5 (2)
C8—N1—C4—C51.2 (3)C22—C23—C24—C251.1 (4)
Re1—N1—C4—C5173.82 (18)C26—C23—C24—C25176.9 (2)
C8—N1—C4—C21177.1 (2)C21—N2—C25—C240.2 (4)
Re1—N1—C4—C214.6 (3)Re1—N2—C25—C24176.83 (18)
N1—C4—C5—C61.2 (4)C23—C24—C25—N21.0 (4)
C21—C4—C5—C6177.0 (2)C22—C23—C26—C274.2 (4)
C4—C5—C6—C70.3 (4)C24—C23—C26—C27173.6 (3)
C4—C5—C6—C9178.6 (2)C23—C26—C27—C28177.5 (2)
C5—C6—C7—C80.5 (4)C26—C27—C28—C335.3 (4)
C9—C6—C7—C8179.3 (2)C26—C27—C28—C29171.7 (3)
C4—N1—C8—C70.4 (4)C33—C28—C29—C300.5 (4)
Re1—N1—C8—C7172.38 (19)C27—C28—C29—C30176.6 (2)
C6—C7—C8—N10.4 (4)C28—C29—C30—C311.1 (4)
C5—C6—C9—C10173.8 (3)C36—N4—C31—C3021.1 (4)
C7—C6—C9—C105.0 (4)C34—N4—C31—C30177.1 (2)
C6—C9—C10—C11174.9 (2)C36—N4—C31—C32159.8 (2)
C9—C10—C11—C16173.4 (3)C34—N4—C31—C322.0 (4)
C9—C10—C11—C126.7 (4)C29—C30—C31—N4178.3 (2)
C16—C11—C12—C132.6 (4)C29—C30—C31—C320.7 (4)
C10—C11—C12—C13177.5 (2)N4—C31—C32—C33179.3 (2)
C11—C12—C13—C140.2 (4)C30—C31—C32—C330.2 (4)
C17—N3—C14—C130.6 (4)C31—C32—C33—C280.8 (4)
C19—N3—C14—C13176.4 (2)C29—C28—C33—C320.5 (4)
C17—N3—C14—C15179.4 (2)C27—C28—C33—C32177.5 (2)
C19—N3—C14—C153.6 (4)C31—N4—C34—C3581.4 (3)
C12—C13—C14—N3178.1 (2)C36—N4—C34—C3580.9 (3)
C12—C13—C14—C151.8 (4)C31—N4—C36—C3764.3 (3)
N3—C14—C15—C16178.6 (2)C34—N4—C36—C3798.2 (3)

Experimental details

Crystal data
Chemical formula[ReCl(C34H38N4)(CO)3]
Mr808.36
Crystal system, space groupMonoclinic, P21/c
Temperature (K)90
a, b, c (Å)14.4908 (5), 23.1755 (5), 9.6971 (5)
β (°) 91.899 (2)
V3)3254.8 (2)
Z4
Radiation typeMo Kα
µ (mm1)3.86
Crystal size (mm)0.3 × 0.2 × 0.1
Data collection
DiffractometerCCD area-detector
diffractometer
Absorption correction(SADABS; Bruker, 1998)
Tmin, Tmax0.391, 0.699
No. of measured, independent and
observed [I > 2σ(I)] reflections
36470, 10508, 8209
Rint0.058
(sin θ/λ)max1)0.756
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.065, 0.97
No. of reflections10508
No. of parameters420
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.75, 1.72

Computer programs: SMART (Bruker, 1998), SMART, SHELXTL (Sheldrick, 1997), SHELXTL.

 

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