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The title compound, [Nb2(μ-Cl)2Cl4(CH3CN)4]·2CH3CN, is a centrosymmetric dinuclear niobium complex containing an NbIII=NbIII double bond [2.8577 (9) Å]. The Nb atom has a distorted octahedral coordination environment formed by two terminal Cl atoms [Nb—Cl = 2.3761 (14) and 2.3853 (15) Å], two aceto­nitrile ligands [Nb—N = 2.301 (4) and 2.309 (4) Å] and two μ-Cl atoms [Nb—Cl = 2.3356 (13) and 2.3358 (13) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804012760/ob6374sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804012760/ob6374Isup2.hkl
Contains datablock I

CCDC reference: 245105

Key indicators

  • Single-crystal X-ray study
  • T = 297 K
  • Mean [sigma](C-C) = 0.012 Å
  • R factor = 0.053
  • wR factor = 0.136
  • Data-to-parameter ratio = 25.4

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb1 - Cl1 .. 7.28 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb1 - Cl1_a .. 8.03 su PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Nb1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C5 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12
0 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 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 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART-W2K/NT (Bruker, 2003); cell refinement: SAINT-W2K/NT (Bruker, 2003); data reduction: SAINT-W2K/NT; program(s) used to solve structure: SHELXTL-NT (Bruker, 2003); program(s) used to refine structure: SHELXTL-NT; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL-NT.

Di-µ-chloro-bis[dichlorobis(acetonitrile)niobium] acetonitorile disolvate top
Crystal data top
[Nb2Cl6(C2H3N)4]·2C2H3NZ = 1
Mr = 644.84F(000) = 316
Triclinic, P1Dx = 1.706 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.331 (2) ÅCell parameters from 1556 reflections
b = 8.997 (2) Åθ = 2.4–27.7°
c = 9.341 (2) ŵ = 1.56 mm1
α = 105.851 (4)°T = 297 K
β = 108.501 (4)°Cubic, black
γ = 94.671 (4)°0.45 × 0.32 × 0.24 mm
V = 627.8 (2) Å3
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
3077 independent reflections
Radiation source: fine-focus sealed tube2457 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
Detector resolution: 8.366 pixels mm-1θmax = 28.3°, θmin = 2.4°
φ and ω scansh = 119
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1111
Tmin = 0.540, Tmax = 0.691l = 1112
4583 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)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.136H-atom parameters constrained
S = 1.06 w = 1/[σ2(Fo2) + (0.0782P)2 + 0.0314P]
where P = (Fo2 + 2Fc2)/3
3077 reflections(Δ/σ)max < 0.001
121 parametersΔρmax = 1.34 e Å3
0 restraintsΔρmin = 0.97 e Å3
Special details top

Experimental. none

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
Nb10.13826 (5)0.63102 (5)0.05878 (5)0.03170 (16)
Cl10.08725 (16)0.40041 (15)0.15203 (15)0.0422 (3)
Cl20.02302 (17)0.78474 (16)0.10604 (17)0.0471 (3)
Cl30.34885 (18)0.55578 (17)0.25367 (16)0.0515 (3)
N10.2219 (6)0.8738 (5)0.2508 (5)0.0477 (11)
N20.3837 (6)0.7181 (5)0.0183 (6)0.0486 (11)
C30.5035 (7)0.7761 (6)0.0090 (7)0.0421 (11)
C10.2497 (8)0.9925 (7)0.3407 (7)0.0553 (15)
C40.6558 (8)0.8499 (8)0.0051 (9)0.0605 (16)
H4A0.70550.77090.05990.091*
H4B0.73780.90580.09900.091*
H4C0.62530.92200.06400.091*
C20.2805 (12)1.1489 (8)0.4560 (9)0.087 (3)
H2A0.26451.22570.40130.130*
H2B0.39631.17260.53090.130*
H2C0.20111.15090.51150.130*
C50.2818 (14)0.7621 (13)0.6234 (9)0.090 (3)
C60.2262 (12)0.5981 (12)0.5846 (11)0.098 (3)
H6A0.16240.55410.47250.147*
H6B0.15390.58020.64270.147*
H6C0.32460.54890.61240.147*
N30.3292 (18)0.8888 (12)0.6568 (12)0.147 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.0283 (2)0.0289 (2)0.0384 (3)0.00031 (15)0.01678 (18)0.00710 (16)
Cl10.0443 (7)0.0389 (6)0.0466 (7)0.0021 (5)0.0274 (6)0.0068 (5)
Cl20.0441 (7)0.0469 (7)0.0641 (8)0.0106 (6)0.0277 (6)0.0282 (6)
Cl30.0416 (7)0.0540 (8)0.0503 (8)0.0056 (6)0.0082 (6)0.0138 (6)
N10.046 (3)0.036 (2)0.051 (3)0.0019 (19)0.015 (2)0.002 (2)
N20.044 (3)0.040 (2)0.068 (3)0.005 (2)0.030 (2)0.016 (2)
C30.037 (3)0.035 (3)0.063 (3)0.010 (2)0.027 (2)0.018 (2)
C10.054 (4)0.042 (3)0.059 (4)0.001 (3)0.013 (3)0.010 (3)
C40.044 (3)0.053 (3)0.098 (5)0.006 (3)0.039 (3)0.031 (3)
C20.112 (7)0.048 (4)0.067 (4)0.013 (4)0.011 (4)0.007 (3)
C50.122 (8)0.104 (7)0.057 (5)0.012 (6)0.048 (5)0.030 (5)
C60.096 (6)0.121 (8)0.085 (6)0.004 (6)0.041 (5)0.041 (6)
N30.243 (14)0.096 (7)0.115 (7)0.019 (8)0.079 (8)0.040 (6)
Geometric parameters (Å, º) top
Nb1—N12.301 (4)C4—H4A0.9600
Nb1—N22.309 (4)C4—H4B0.9600
Nb1—Cl1i2.3356 (13)C4—H4C0.9600
Nb1—Cl12.3358 (13)C2—H2A0.9600
Nb1—Cl22.3761 (14)C2—H2B0.9600
Nb1—Cl32.3853 (15)C2—H2C0.9600
Nb1—Nb1i2.8577 (9)C5—N31.098 (12)
N1—C11.116 (7)C5—C61.419 (13)
N2—C31.127 (7)C6—H6A0.9600
C3—C41.444 (7)C6—H6B0.9600
C1—C21.464 (9)C6—H6C0.9600
N1—Nb1—N281.22 (17)C3—N2—Nb1172.5 (4)
N1—Nb1—Cl1i84.86 (12)N2—C3—C4179.2 (7)
N2—Nb1—Cl1i166.01 (12)N1—C1—C2178.2 (7)
N1—Nb1—Cl1170.38 (12)C3—C4—H4A109.5
N2—Nb1—Cl189.39 (12)C3—C4—H4B109.5
Cl1i—Nb1—Cl1104.57 (4)H4A—C4—H4B109.5
N1—Nb1—Cl281.48 (13)C3—C4—H4C109.5
N2—Nb1—Cl280.67 (12)H4A—C4—H4C109.5
Cl1i—Nb1—Cl298.70 (5)H4B—C4—H4C109.5
Cl1—Nb1—Cl294.97 (5)C1—C2—H2A109.5
N1—Nb1—Cl383.93 (13)C1—C2—H2B109.5
N2—Nb1—Cl380.18 (13)H2A—C2—H2B109.5
Cl1i—Nb1—Cl397.01 (5)C1—C2—H2C109.5
Cl1—Nb1—Cl396.63 (5)H2A—C2—H2C109.5
Cl2—Nb1—Cl3157.44 (5)H2B—C2—H2C109.5
N1—Nb1—Nb1i137.11 (12)N3—C5—C6177.9 (13)
N2—Nb1—Nb1i141.66 (12)C5—C6—H6A109.5
Cl1i—Nb1—Nb1i52.29 (3)C5—C6—H6B109.5
Cl1—Nb1—Nb1i52.28 (3)H6A—C6—H6B109.5
Cl2—Nb1—Nb1i101.21 (4)C5—C6—H6C109.5
Cl3—Nb1—Nb1i101.20 (4)H6A—C6—H6C109.5
Nb1i—Cl1—Nb175.43 (4)H6B—C6—H6C109.5
C1—N1—Nb1174.7 (5)
Cl1i—Nb1—Cl1—Nb1i0.0Cl3—Nb1—Cl1—Nb1i99.05 (5)
Cl2—Nb1—Cl1—Nb1i100.34 (5)
Symmetry code: (i) x, y+1, z.
 

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