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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
CCDC reference: 245105
Key indicators
- Single-crystal X-ray study
- T = 297 K
- Mean (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
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]·2C2H3N | Z = 1 |
Mr = 644.84 | F(000) = 316 |
Triclinic, P1 | Dx = 1.706 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.331 (2) Å | Cell parameters from 1556 reflections |
b = 8.997 (2) Å | θ = 2.4–27.7° |
c = 9.341 (2) Å | µ = 1.56 mm−1 |
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 tube | 2457 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
Detector resolution: 8.366 pixels mm-1 | θmax = 28.3°, θmin = 2.4° |
φ and ω scans | h = −11→9 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −11→11 |
Tmin = 0.540, Tmax = 0.691 | l = −11→12 |
4583 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.136 | H-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 parameters | Δρmax = 1.34 e Å−3 |
0 restraints | Δρmin = −0.97 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Nb1 | 0.13826 (5) | 0.63102 (5) | 0.05878 (5) | 0.03170 (16) | |
Cl1 | 0.08725 (16) | 0.40041 (15) | −0.15203 (15) | 0.0422 (3) | |
Cl2 | 0.02302 (17) | 0.78474 (16) | −0.10604 (17) | 0.0471 (3) | |
Cl3 | 0.34885 (18) | 0.55578 (17) | 0.25367 (16) | 0.0515 (3) | |
N1 | 0.2219 (6) | 0.8738 (5) | 0.2508 (5) | 0.0477 (11) | |
N2 | 0.3837 (6) | 0.7181 (5) | 0.0183 (6) | 0.0486 (11) | |
C3 | 0.5035 (7) | 0.7761 (6) | 0.0090 (7) | 0.0421 (11) | |
C1 | 0.2497 (8) | 0.9925 (7) | 0.3407 (7) | 0.0553 (15) | |
C4 | 0.6558 (8) | 0.8499 (8) | −0.0051 (9) | 0.0605 (16) | |
H4A | 0.7055 | 0.7709 | −0.0599 | 0.091* | |
H4B | 0.7378 | 0.9058 | 0.0990 | 0.091* | |
H4C | 0.6253 | 0.9220 | −0.0640 | 0.091* | |
C2 | 0.2805 (12) | 1.1489 (8) | 0.4560 (9) | 0.087 (3) | |
H2A | 0.2645 | 1.2257 | 0.4013 | 0.130* | |
H2B | 0.3963 | 1.1726 | 0.5309 | 0.130* | |
H2C | 0.2011 | 1.1509 | 0.5115 | 0.130* | |
C5 | 0.2818 (14) | 0.7621 (13) | 0.6234 (9) | 0.090 (3) | |
C6 | 0.2262 (12) | 0.5981 (12) | 0.5846 (11) | 0.098 (3) | |
H6A | 0.1624 | 0.5541 | 0.4725 | 0.147* | |
H6B | 0.1539 | 0.5802 | 0.6427 | 0.147* | |
H6C | 0.3246 | 0.5489 | 0.6124 | 0.147* | |
N3 | 0.3292 (18) | 0.8888 (12) | 0.6568 (12) | 0.147 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nb1 | 0.0283 (2) | 0.0289 (2) | 0.0384 (3) | −0.00031 (15) | 0.01678 (18) | 0.00710 (16) |
Cl1 | 0.0443 (7) | 0.0389 (6) | 0.0466 (7) | 0.0021 (5) | 0.0274 (6) | 0.0068 (5) |
Cl2 | 0.0441 (7) | 0.0469 (7) | 0.0641 (8) | 0.0106 (6) | 0.0277 (6) | 0.0282 (6) |
Cl3 | 0.0416 (7) | 0.0540 (8) | 0.0503 (8) | 0.0056 (6) | 0.0082 (6) | 0.0138 (6) |
N1 | 0.046 (3) | 0.036 (2) | 0.051 (3) | −0.0019 (19) | 0.015 (2) | 0.002 (2) |
N2 | 0.044 (3) | 0.040 (2) | 0.068 (3) | 0.005 (2) | 0.030 (2) | 0.016 (2) |
C3 | 0.037 (3) | 0.035 (3) | 0.063 (3) | 0.010 (2) | 0.027 (2) | 0.018 (2) |
C1 | 0.054 (4) | 0.042 (3) | 0.059 (4) | 0.001 (3) | 0.013 (3) | 0.010 (3) |
C4 | 0.044 (3) | 0.053 (3) | 0.098 (5) | 0.006 (3) | 0.039 (3) | 0.031 (3) |
C2 | 0.112 (7) | 0.048 (4) | 0.067 (4) | 0.013 (4) | 0.011 (4) | −0.007 (3) |
C5 | 0.122 (8) | 0.104 (7) | 0.057 (5) | 0.012 (6) | 0.048 (5) | 0.030 (5) |
C6 | 0.096 (6) | 0.121 (8) | 0.085 (6) | −0.004 (6) | 0.041 (5) | 0.041 (6) |
N3 | 0.243 (14) | 0.096 (7) | 0.115 (7) | 0.019 (8) | 0.079 (8) | 0.040 (6) |
Geometric parameters (Å, º) top
Nb1—N1 | 2.301 (4) | C4—H4A | 0.9600 |
Nb1—N2 | 2.309 (4) | C4—H4B | 0.9600 |
Nb1—Cl1i | 2.3356 (13) | C4—H4C | 0.9600 |
Nb1—Cl1 | 2.3358 (13) | C2—H2A | 0.9600 |
Nb1—Cl2 | 2.3761 (14) | C2—H2B | 0.9600 |
Nb1—Cl3 | 2.3853 (15) | C2—H2C | 0.9600 |
Nb1—Nb1i | 2.8577 (9) | C5—N3 | 1.098 (12) |
N1—C1 | 1.116 (7) | C5—C6 | 1.419 (13) |
N2—C3 | 1.127 (7) | C6—H6A | 0.9600 |
C3—C4 | 1.444 (7) | C6—H6B | 0.9600 |
C1—C2 | 1.464 (9) | C6—H6C | 0.9600 |
| | | |
N1—Nb1—N2 | 81.22 (17) | C3—N2—Nb1 | 172.5 (4) |
N1—Nb1—Cl1i | 84.86 (12) | N2—C3—C4 | 179.2 (7) |
N2—Nb1—Cl1i | 166.01 (12) | N1—C1—C2 | 178.2 (7) |
N1—Nb1—Cl1 | 170.38 (12) | C3—C4—H4A | 109.5 |
N2—Nb1—Cl1 | 89.39 (12) | C3—C4—H4B | 109.5 |
Cl1i—Nb1—Cl1 | 104.57 (4) | H4A—C4—H4B | 109.5 |
N1—Nb1—Cl2 | 81.48 (13) | C3—C4—H4C | 109.5 |
N2—Nb1—Cl2 | 80.67 (12) | H4A—C4—H4C | 109.5 |
Cl1i—Nb1—Cl2 | 98.70 (5) | H4B—C4—H4C | 109.5 |
Cl1—Nb1—Cl2 | 94.97 (5) | C1—C2—H2A | 109.5 |
N1—Nb1—Cl3 | 83.93 (13) | C1—C2—H2B | 109.5 |
N2—Nb1—Cl3 | 80.18 (13) | H2A—C2—H2B | 109.5 |
Cl1i—Nb1—Cl3 | 97.01 (5) | C1—C2—H2C | 109.5 |
Cl1—Nb1—Cl3 | 96.63 (5) | H2A—C2—H2C | 109.5 |
Cl2—Nb1—Cl3 | 157.44 (5) | H2B—C2—H2C | 109.5 |
N1—Nb1—Nb1i | 137.11 (12) | N3—C5—C6 | 177.9 (13) |
N2—Nb1—Nb1i | 141.66 (12) | C5—C6—H6A | 109.5 |
Cl1i—Nb1—Nb1i | 52.29 (3) | C5—C6—H6B | 109.5 |
Cl1—Nb1—Nb1i | 52.28 (3) | H6A—C6—H6B | 109.5 |
Cl2—Nb1—Nb1i | 101.21 (4) | C5—C6—H6C | 109.5 |
Cl3—Nb1—Nb1i | 101.20 (4) | H6A—C6—H6C | 109.5 |
Nb1i—Cl1—Nb1 | 75.43 (4) | H6B—C6—H6C | 109.5 |
C1—N1—Nb1 | 174.7 (5) | | |
| | | |
Cl1i—Nb1—Cl1—Nb1i | 0.0 | Cl3—Nb1—Cl1—Nb1i | 99.05 (5) |
Cl2—Nb1—Cl1—Nb1i | −100.34 (5) | | |
Symmetry code: (i) −x, −y+1, −z. |
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