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The title compound, (C8H20N)[Nb(C6H4S2)2(C6H4S3)], is the major product of the reaction of (Et4N)4[Nb2S4(NCS)8] and disodium benzene-1,2-di­thiol­ate. The coordination environment of the Nb atom contains seven S atoms, viz. four S atoms from two benzene-1,2-di­thiol­ate ligands and three S atoms from 2-disulfanyl­benzene­thiol­ate. The Nb-S distances are in the range 2.4391 (6)-2.5932 (7) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805012869/cv6492sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805012869/cv6492Isup2.hkl
Contains datablock I

CCDC reference: 274376

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.031
  • wR factor = 0.082
  • Data-to-parameter ratio = 16.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.86 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT223_ALERT_4_C Large Solvent/Anion H Ueq(max)/Ueq(min) ... 3.47 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb1 - S11 .. 8.42 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb1 - S22 .. 5.59 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb1 - S31 .. 5.06 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Nb1 - S32 .. 6.19 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C2 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.08
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 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 6 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2004); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Tetraethylammonium bis(benzene-1,2-dithiolato)(2-disulfanylbenzenethiolato)niobate top
Crystal data top
(C8H20N)[Nb(C6H4S2)2(C6H4S3)]F(000) = 1392
Mr = 675.86Dx = 1.537 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 10.8255 (3) ÅCell parameters from 6454 reflections
b = 17.9119 (5) Åθ = 2.6–30.7°
c = 15.0647 (4) ŵ = 0.93 mm1
β = 90.423 (1)°T = 150 K
V = 2921.05 (14) Å3Prism, black
Z = 40.30 × 0.20 × 0.15 mm
Data collection top
Bruker Nonius X8Apex CCD area-detector
diffractometer
5338 independent reflections
Radiation source: fine-focus sealed tube4345 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
Detector resolution: 25 pixels mm-1θmax = 25.4°, θmin = 1.8°
φ scansh = 1213
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
k = 2120
Tmin = 0.768, Tmax = 0.873l = 1813
17313 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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.082H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0517P)2 + 0.018P]
where P = (Fo2 + 2Fc2)/3
5338 reflections(Δ/σ)max = 0.001
320 parametersΔρmax = 1.11 e Å3
0 restraintsΔρmin = 0.29 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
Nb10.276664 (19)0.351406 (11)0.179997 (13)0.02481 (9)
S110.12893 (6)0.25436 (4)0.22293 (4)0.03115 (16)
S120.23502 (5)0.29041 (3)0.03105 (4)0.02959 (15)
S210.36660 (6)0.34492 (3)0.33088 (4)0.03270 (16)
S220.48293 (6)0.29881 (3)0.14780 (4)0.03092 (15)
S310.36947 (5)0.44665 (3)0.08493 (4)0.02857 (15)
S320.08351 (6)0.43300 (4)0.14807 (4)0.03368 (16)
S330.16690 (6)0.44227 (3)0.27064 (4)0.03443 (16)
N10.39606 (19)0.06057 (11)0.20798 (14)0.0349 (5)
C10.2050 (3)0.0021 (2)0.2715 (3)0.0927 (14)
H1A0.19690.02960.32410.139*
H1B0.17120.05170.28420.139*
H1C0.15950.02030.22180.139*
C20.3391 (2)0.00915 (15)0.2478 (2)0.0467 (7)
H2A0.34810.05070.20490.056*
H2B0.38630.02270.30200.056*
C30.3217 (3)0.02498 (18)0.0519 (2)0.0627 (9)
H3A0.40540.00970.03540.094*
H3B0.27900.04560.00020.094*
H3C0.27600.01840.07390.094*
C40.3290 (3)0.08392 (16)0.12398 (19)0.0467 (7)
H4A0.37090.12850.09950.056*
H4B0.24390.09890.13970.056*
C50.4572 (4)0.11939 (18)0.35789 (19)0.0638 (10)
H5A0.43180.07350.38800.096*
H5B0.43950.16250.39580.096*
H5C0.54600.11740.34590.096*
C60.3868 (3)0.12693 (15)0.27127 (19)0.0476 (8)
H6A0.41710.17200.24010.057*
H6B0.29860.13530.28490.057*
C70.6073 (3)0.10266 (16)0.15322 (19)0.0482 (7)
H7A0.57180.11920.09650.072*
H7B0.69160.08450.14380.072*
H7C0.60910.14460.19490.072*
C80.5295 (2)0.04068 (14)0.19072 (17)0.0335 (6)
H8A0.56760.02390.24720.040*
H8B0.53150.00200.14900.040*
C110.0747 (2)0.20515 (13)0.12988 (15)0.0263 (5)
C120.1246 (2)0.22002 (13)0.04570 (15)0.0258 (5)
C130.0854 (2)0.17657 (14)0.02626 (15)0.0309 (5)
H130.11620.18690.08390.037*
C140.0028 (2)0.11907 (15)0.01475 (17)0.0370 (6)
H140.02180.08960.06430.044*
C150.0451 (2)0.10359 (14)0.06883 (17)0.0363 (6)
H150.10120.06340.07670.044*
C160.0098 (2)0.14759 (13)0.14050 (17)0.0326 (6)
H160.04390.13820.19740.039*
C210.5217 (2)0.31742 (14)0.32552 (17)0.0348 (6)
C220.5752 (2)0.30164 (13)0.24401 (16)0.0327 (6)
C230.7015 (2)0.28495 (15)0.2412 (2)0.0440 (7)
H230.73910.27350.18600.053*
C240.7718 (3)0.28504 (17)0.3180 (2)0.0546 (8)
H240.85780.27480.31520.065*
C250.7178 (3)0.29989 (17)0.3987 (2)0.0560 (8)
H250.76650.29970.45150.067*
C260.5936 (3)0.31499 (16)0.40291 (19)0.0470 (7)
H260.55630.32390.45880.056*
C310.2587 (2)0.51494 (13)0.05826 (15)0.0306 (5)
C320.1375 (2)0.51232 (14)0.08890 (16)0.0338 (6)
C330.0551 (2)0.57017 (15)0.07151 (18)0.0432 (7)
H330.02730.56760.09270.052*
C340.0937 (3)0.63137 (16)0.0232 (2)0.0493 (8)
H340.03870.67170.01220.059*
C350.2125 (3)0.63365 (15)0.00900 (19)0.0461 (7)
H350.23820.67530.04330.055*
C360.2945 (2)0.57650 (14)0.00779 (16)0.0377 (6)
H360.37590.57900.01510.045*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nb10.02565 (13)0.02397 (13)0.02490 (14)0.00080 (8)0.00548 (9)0.00016 (8)
S110.0349 (3)0.0326 (3)0.0260 (3)0.0065 (3)0.0079 (3)0.0006 (2)
S120.0300 (3)0.0336 (3)0.0252 (3)0.0044 (3)0.0059 (2)0.0004 (3)
S210.0378 (4)0.0340 (4)0.0263 (3)0.0031 (3)0.0020 (3)0.0009 (3)
S220.0298 (3)0.0317 (3)0.0313 (3)0.0048 (3)0.0044 (3)0.0025 (3)
S310.0277 (3)0.0273 (3)0.0308 (3)0.0003 (2)0.0083 (3)0.0023 (2)
S320.0267 (3)0.0354 (4)0.0390 (4)0.0018 (3)0.0075 (3)0.0027 (3)
S330.0397 (4)0.0315 (3)0.0322 (3)0.0019 (3)0.0113 (3)0.0026 (3)
N10.0324 (12)0.0292 (11)0.0431 (13)0.0079 (9)0.0124 (10)0.0086 (9)
C10.051 (2)0.071 (3)0.157 (4)0.0073 (19)0.046 (2)0.046 (3)
C20.0428 (16)0.0345 (15)0.0630 (19)0.0021 (13)0.0180 (14)0.0181 (14)
C30.061 (2)0.063 (2)0.064 (2)0.0054 (17)0.0198 (17)0.0087 (17)
C40.0382 (16)0.0425 (17)0.0595 (19)0.0108 (13)0.0010 (13)0.0166 (14)
C50.106 (3)0.0465 (19)0.0394 (18)0.0181 (19)0.0186 (18)0.0015 (14)
C60.0580 (19)0.0342 (15)0.0510 (18)0.0155 (14)0.0265 (15)0.0097 (13)
C70.0402 (16)0.0489 (18)0.0557 (18)0.0026 (13)0.0178 (14)0.0067 (14)
C80.0302 (13)0.0359 (14)0.0344 (14)0.0091 (11)0.0066 (11)0.0024 (11)
C110.0229 (12)0.0275 (13)0.0286 (13)0.0035 (10)0.0018 (10)0.0015 (10)
C120.0222 (12)0.0279 (13)0.0275 (12)0.0046 (10)0.0016 (9)0.0008 (10)
C130.0277 (13)0.0354 (14)0.0298 (13)0.0045 (11)0.0002 (10)0.0016 (11)
C140.0311 (14)0.0400 (15)0.0399 (15)0.0001 (12)0.0034 (11)0.0110 (12)
C150.0285 (14)0.0341 (14)0.0462 (16)0.0087 (11)0.0026 (11)0.0046 (12)
C160.0257 (13)0.0361 (14)0.0362 (14)0.0020 (11)0.0068 (11)0.0018 (11)
C210.0383 (15)0.0259 (13)0.0402 (15)0.0077 (11)0.0051 (11)0.0007 (11)
C220.0323 (14)0.0269 (13)0.0387 (14)0.0041 (10)0.0033 (11)0.0056 (11)
C230.0336 (15)0.0402 (16)0.0583 (19)0.0001 (12)0.0004 (13)0.0040 (13)
C240.0330 (16)0.055 (2)0.076 (2)0.0023 (14)0.0161 (15)0.0051 (16)
C250.052 (2)0.054 (2)0.062 (2)0.0072 (15)0.0252 (16)0.0018 (16)
C260.0522 (19)0.0460 (17)0.0427 (16)0.0053 (14)0.0133 (13)0.0028 (13)
C310.0342 (14)0.0301 (13)0.0275 (12)0.0015 (11)0.0032 (10)0.0007 (10)
C320.0326 (14)0.0318 (14)0.0369 (14)0.0023 (11)0.0003 (11)0.0030 (11)
C330.0317 (15)0.0483 (17)0.0497 (17)0.0065 (13)0.0021 (12)0.0053 (14)
C340.0502 (19)0.0427 (17)0.0551 (19)0.0166 (14)0.0071 (15)0.0084 (14)
C350.0524 (19)0.0401 (16)0.0457 (17)0.0021 (14)0.0008 (14)0.0142 (13)
C360.0408 (15)0.0386 (15)0.0338 (14)0.0005 (12)0.0071 (12)0.0068 (12)
Geometric parameters (Å, º) top
Nb1—S112.4522 (6)C7—C81.506 (4)
Nb1—S122.5331 (6)C7—H7A0.9800
Nb1—S212.4688 (6)C7—H7B0.9800
Nb1—S222.4748 (6)C7—H7C0.9800
Nb1—S312.4479 (6)C8—H8A0.9900
Nb1—S322.5932 (7)C8—H8B0.9900
Nb1—S332.4391 (6)C11—C161.388 (3)
S11—C111.753 (2)C11—C121.408 (3)
S12—C121.752 (2)C12—C131.398 (3)
S21—C211.753 (3)C13—C141.376 (4)
S22—C221.755 (3)C13—H130.9500
S31—C311.757 (2)C14—C151.393 (3)
S32—C321.779 (2)C14—H140.9500
S32—S332.0561 (9)C15—C161.388 (3)
N1—C81.513 (3)C15—H150.9500
N1—C41.513 (3)C16—H160.9500
N1—C21.518 (3)C21—C221.390 (3)
N1—C61.528 (3)C21—C261.397 (4)
C1—C21.502 (4)C22—C231.401 (4)
C1—H1A0.9800C23—C241.380 (4)
C1—H1B0.9800C23—H230.9500
C1—H1C0.9800C24—C251.379 (4)
C2—H2A0.9900C24—H240.9500
C2—H2B0.9900C25—C261.373 (4)
C3—C41.516 (4)C25—H250.9500
C3—H3A0.9800C26—H260.9500
C3—H3B0.9800C31—C321.395 (3)
C3—H3C0.9800C31—C361.396 (3)
C4—H4A0.9900C32—C331.391 (3)
C4—H4B0.9900C33—C341.383 (4)
C5—C61.512 (4)C33—H330.9500
C5—H5A0.9800C34—C351.378 (4)
C5—H5B0.9800C34—H340.9500
C5—H5C0.9800C35—C361.377 (4)
C6—H6A0.9900C35—H350.9500
C6—H6B0.9900C36—H360.9500
S11—Nb1—S1279.38 (2)C5—C6—H6B108.3
S21—Nb1—S2279.18 (2)N1—C6—H6B108.3
S31—Nb1—S3280.36 (2)H6A—C6—H6B107.4
S31—Nb1—S3393.80 (2)C8—C7—H7A109.5
S32—Nb1—S3348.11 (2)C8—C7—H7B109.5
S33—Nb1—S1190.23 (2)H7A—C7—H7B109.5
S31—Nb1—S11156.88 (2)C8—C7—H7C109.5
S33—Nb1—S2172.93 (2)H7A—C7—H7C109.5
S31—Nb1—S21114.25 (2)H7B—C7—H7C109.5
S11—Nb1—S2188.70 (2)C7—C8—N1115.4 (2)
S33—Nb1—S22143.87 (2)C7—C8—H8A108.4
S31—Nb1—S2277.05 (2)N1—C8—H8A108.4
S11—Nb1—S22111.90 (2)C7—C8—H8B108.4
S33—Nb1—S12134.38 (2)N1—C8—H8B108.4
S31—Nb1—S1281.58 (2)H8A—C8—H8B107.5
S21—Nb1—S12149.50 (2)C16—C11—C12120.1 (2)
S22—Nb1—S1279.47 (2)C16—C11—S11119.88 (18)
S11—Nb1—S3285.52 (2)C12—C11—S11119.77 (17)
S21—Nb1—S32120.61 (2)C13—C12—C11118.5 (2)
S22—Nb1—S32154.91 (2)C13—C12—S12120.42 (17)
S12—Nb1—S3286.61 (2)C11—C12—S12121.09 (17)
C11—S11—Nb1111.14 (8)C14—C13—C12120.9 (2)
C12—S12—Nb1108.41 (8)C14—C13—H13119.6
C21—S21—Nb1110.02 (9)C12—C13—H13119.6
C22—S22—Nb1109.64 (9)C13—C14—C15120.6 (2)
C31—S31—Nb1109.67 (8)C13—C14—H14119.7
C32—S32—S33103.99 (9)C15—C14—H14119.7
C32—S32—Nb1105.99 (8)C16—C15—C14119.2 (2)
S33—S32—Nb162.02 (2)C16—C15—H15120.4
S32—S33—Nb169.87 (2)C14—C15—H15120.4
C8—N1—C4111.97 (19)C15—C16—C11120.6 (2)
C8—N1—C2105.41 (18)C15—C16—H16119.7
C4—N1—C2111.3 (2)C11—C16—H16119.7
C8—N1—C6111.0 (2)C22—C21—C26119.9 (3)
C4—N1—C6105.89 (19)C22—C21—S21120.20 (19)
C2—N1—C6111.39 (19)C26—C21—S21119.9 (2)
C2—C1—H1A109.5C21—C22—C23118.9 (2)
C2—C1—H1B109.5C21—C22—S22119.81 (19)
H1A—C1—H1B109.5C23—C22—S22121.3 (2)
C2—C1—H1C109.5C24—C23—C22120.4 (3)
H1A—C1—H1C109.5C24—C23—H23119.8
H1B—C1—H1C109.5C22—C23—H23119.8
C1—C2—N1114.9 (2)C25—C24—C23120.3 (3)
C1—C2—H2A108.5C25—C24—H24119.8
N1—C2—H2A108.5C23—C24—H24119.8
C1—C2—H2B108.5C26—C25—C24120.0 (3)
N1—C2—H2B108.5C26—C25—H25120.0
H2A—C2—H2B107.5C24—C25—H25120.0
C4—C3—H3A109.5C25—C26—C21120.5 (3)
C4—C3—H3B109.5C25—C26—H26119.8
H3A—C3—H3B109.5C21—C26—H26119.8
C4—C3—H3C109.5C32—C31—C36118.2 (2)
H3A—C3—H3C109.5C32—C31—S31122.88 (19)
H3B—C3—H3C109.5C36—C31—S31118.86 (19)
N1—C4—C3115.4 (2)C33—C32—C31121.1 (2)
N1—C4—H4A108.4C33—C32—S32118.46 (19)
C3—C4—H4A108.4C31—C32—S32120.41 (19)
N1—C4—H4B108.4C34—C33—C32119.5 (3)
C3—C4—H4B108.4C34—C33—H33120.2
H4A—C4—H4B107.5C32—C33—H33120.2
C6—C5—H5A109.5C35—C34—C33119.7 (3)
C6—C5—H5B109.5C35—C34—H34120.1
H5A—C5—H5B109.5C33—C34—H34120.1
C6—C5—H5C109.5C36—C35—C34121.0 (3)
H5A—C5—H5C109.5C36—C35—H35119.5
H5B—C5—H5C109.5C34—C35—H35119.5
C5—C6—N1115.7 (2)C35—C36—C31120.4 (2)
C5—C6—H6A108.3C35—C36—H36119.8
N1—C6—H6A108.3C31—C36—H36119.8
 

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