(C7H6NS)2[Nb6Cl18]·2C4H8O: first niobium cluster with an N,S-heterocyclic cation

Sperlich, E.; Köckerling, M.

doi:10.1107/S2414314618017601

(C₇H₆NS)₂[Nb₆Cl₁₈]·2C₄H₈O: first niobium cluster with an N,S-heterocyclic cation

The title compound bis(benzothiazolium) dodeca-μ-chlorido-hexachlorido-octahedro-hexaniobium(12 Nb—Nb) tetrahydrofuran disolvate, (C₇H₆NS)₂[Nb₆Cl₁₈]·2C₄H₈O or (HBTh)₂[Nb₆Cl₁₈]·2THF, is the first known niobium cluster compound to contain an N,S-heterocyclic cation. The synthesis takes place within a few hours as an one-pot reaction at room temperature of the cluster precursor compound [Nb₆Cl₁₄(H₂O)₄]·4H₂O with SOCl₂ in the presence of BTh (benzothiazole) in very high yield. The stabilization of the acidic proton of the cation is achieved by the use of tetrahydrofuran as a co-solvent and by the formation of hydrogen bonds.

Keywords: crystal structure; niobium; cluster; dehydration; halides.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314618017601/zq4033sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2414314618017601/zq4033Isup2.hkl Contains datablock I

CCDC reference: 1884787

checkCIF report

Key indicators

Single-crystal X-ray study
T = 123 K
Mean (C-C) = 0.006 Å
Disorder in solvent or counterion
R factor = 0.023
wR factor = 0.047
Data-to-parameter ratio = 19.1

checkCIF/PLATON results

No syntax errors found



Alert level C
ABSMU01_ALERT_1_C  The ratio of given/expected absorption coefficient lies
               outside the range 0.99 <> 1.01
            Calculated value of mu =     2.641
            Value of mu given      =     2.607
PLAT051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       1.30 %
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.8 Note
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.5 Note
PLAT431_ALERT_2_C Short Inter HL..A Contact  Cl8      ..S1       .       3.33 Ang.
                                                 1-x,1-y,-z  =      3_665 Check

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         10 Note
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...         10 Report
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       5.19 Why ?
PLAT152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ...         -5 Units
PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          3 Report
PLAT178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records          2 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Nb1      --Cl2      .        5.7 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Nb1      --Cl4      .        6.0 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Nb1      --Cl6_a    .        5.7 s.u.
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  3  )       100% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  4  )       100% Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  3          7.28 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  4          5.72 Check
PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.34 Ratio
PLAT794_ALERT_5_G Tentative Bond Valency for Nb1       (III)     .       2.64 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Nb2       (III)     .       2.65 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Nb3       (III)     .       2.61 Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         86 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          2 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          5 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          8 Info
PLAT982_ALERT_1_G The Cl-f'=    0.1507 Deviates from  IT-value =       0.1484Check
PLAT982_ALERT_1_G The Nb-f'=   -2.0614 Deviates from  IT-value =      -2.0727Check
PLAT982_ALERT_1_G The  S-f'=    0.1265 Deviates from  IT-value =       0.1246Check
PLAT983_ALERT_1_G The Cl-f"=    0.1611 Deviates from  IT-Value =       0.1585Check
PLAT983_ALERT_1_G The Nb-f"=    0.6336 Deviates from  IT-Value =       0.6215Check
PLAT983_ALERT_1_G The  S-f"=    0.1256 Deviates from  IT-Value =       0.1234Check

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   5 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  28 ALERT level G = General information/check it is not something unexpected

  10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  10 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   8 ALERT type 4 Improvement, methodology, query or suggestion
   3 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX3 (Bruker, 2017); cell refinement: SAINT (Bruker, 2017); data reduction: SAINT (Bruker, 2017); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: SHELXTL (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2014); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Bis(benzothiazolium) dodeca-µ-chlorido-hexachlorido-octahedro-hexaniobium(12 Nb—Nb) tetrahydrofuran disolvate top

Crystal data top

(C₇H₆NS)₂[Nb₆Cl₁₈]·2C₄H₈O	F(000) = 1548
M_r = 1612.14	D_x = 2.355 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 8.7110 (3) Å	Cell parameters from 9607 reflections
b = 24.171 (1) Å	θ = 2.4–27.9°
c = 11.0653 (4) Å	µ = 2.61 mm⁻¹
β = 102.598 (1)°	T = 123 K
V = 2273.8 (2) Å³	Block, brown
Z = 2	0.20 × 0.15 × 0.15 mm

Data collection top

Bruker APEXII CCD diffractometer	4867 reflections with I > 2σ(I)
Radiation source: microfocus sealed tube	R_int = 0.045
φ and ω scans	θ_max = 27.9°, θ_min = 2.4°
Absorption correction: multi-scan (SADABS; Bruker, 2017)	h = −11→11
	k = −31→31
102833 measured reflections	l = −14→14
5454 independent reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.023	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.047	w = 1/[σ²(F_o²) + (0.0133P)² + 5.1918P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.003
5454 reflections	Δρ_max = 1.25 e Å⁻³
286 parameters	Δρ_min = −1.00 e Å⁻³
86 restraints	Extinction correction: SHELXL2014 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00216 (7)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Nb1	0.16489 (2)	0.43379 (2)	0.54806 (2)	0.01537 (6)
Nb2	−0.17270 (2)	0.44311 (2)	0.40346 (2)	0.01362 (6)
Nb3	0.08185 (2)	0.51378 (2)	0.33389 (2)	0.01343 (6)
Cl1	−0.00984 (7)	0.36126 (3)	0.44714 (6)	0.0230 (1)
Cl2	0.27598 (7)	0.44047 (3)	0.36589 (6)	0.0229 (1)
Cl3	0.35309 (8)	0.35643 (3)	0.60609 (8)	0.0366 (2)
Cl4	0.09382 (7)	0.40977 (3)	0.74224 (6)	0.0223 (1)
Cl5	−0.10366 (8)	0.45219 (3)	0.20332 (5)	0.0257 (2)
Cl6	−0.38072 (7)	0.51032 (3)	0.34026 (6)	0.0235 (1)
Cl7	−0.36886 (8)	0.37615 (3)	0.29128 (6)	0.0278 (2)
Cl8	0.17478 (8)	0.53147 (3)	0.13888 (6)	0.0303 (2)
Cl9	0.28546 (6)	0.57995 (2)	0.42073 (5)	0.0157 (1)
S1	0.4979 (1)	0.43271 (4)	−0.04878 (8)	0.0383 (2)
N1	0.3389 (3)	0.3668 (1)	0.0501 (2)	0.0333 (6)
H1A	0.273 (5)	0.356 (2)	0.089 (4)	0.05 (1)*
C1	0.3572 (4)	0.4193 (1)	0.0308 (3)	0.0310 (7)
H1B	0.2971	0.4474	0.0589	0.037*
C2	0.5361 (4)	0.3627 (2)	−0.0584 (3)	0.0369 (8)
C3	0.6409 (5)	0.3356 (2)	−0.1173 (3)	0.050 (1)
H3	0.7055	0.3557	−0.1609	0.060*
C4	0.6474 (5)	0.2793 (2)	−0.1103 (4)	0.059 (1)
H4	0.7164	0.2600	−0.1512	0.071*
C5	0.5551 (6)	0.2490 (2)	−0.0442 (4)	0.063 (1)
H5	0.5659	0.2099	−0.0384	0.076*
C6	0.4500 (5)	0.2751 (2)	0.0121 (4)	0.057 (1)
H6	0.3864	0.2547	0.0559	0.068*
C7	0.4395 (4)	0.3324 (1)	0.0030 (3)	0.0378 (8)
O1A	0.1371 (5)	0.3338 (2)	0.1885 (4)	0.034 (1)	0.560 (9)
C8A	−0.0116 (7)	0.3094 (2)	0.1260 (5)	0.038 (1)	0.560 (9)
H8A	−0.0305	0.3156	0.0355	0.046*	0.560 (9)
H8B	−0.0999	0.3256	0.1572	0.046*	0.560 (9)
C9A	0.0044 (6)	0.2488 (2)	0.1553 (5)	0.040 (1)	0.560 (9)
H9A	−0.0972	0.2332	0.1654	0.048*	0.560 (9)
H9B	0.0393	0.2284	0.0885	0.048*	0.560 (9)
C10A	0.1238 (7)	0.2450 (2)	0.2726 (6)	0.038 (1)	0.560 (9)
H10A	0.1850	0.2103	0.2756	0.046*	0.560 (9)
H10B	0.0732	0.2458	0.3445	0.046*	0.560 (9)
C11A	0.2283 (6)	0.2943 (2)	0.2740 (5)	0.034 (1)	0.560 (9)
H11A	0.2578	0.3103	0.3583	0.041*	0.560 (9)
H11B	0.3254	0.2839	0.2469	0.041*	0.560 (9)
O1B	0.1404 (9)	0.3237 (3)	0.1642 (7)	0.062 (2)	0.440 (9)
C8B	−0.0152 (9)	0.3084 (3)	0.0947 (7)	0.063 (2)	0.440 (9)
H8C	−0.0089	0.2916	0.0142	0.076*	0.440 (9)
H8D	−0.0848	0.3412	0.0790	0.076*	0.440 (9)
C9B	−0.0757 (8)	0.2673 (3)	0.1745 (7)	0.063 (2)	0.440 (9)
H9C	−0.1426	0.2858	0.2241	0.075*	0.440 (9)
H9D	−0.1384	0.2382	0.1231	0.075*	0.440 (9)
C10B	0.066 (1)	0.2432 (3)	0.2560 (8)	0.062 (2)	0.440 (9)
H10C	0.0982	0.2091	0.2188	0.075*	0.440 (9)
H10D	0.0444	0.2340	0.3380	0.075*	0.440 (9)
C11B	0.1908 (8)	0.2866 (4)	0.2683 (8)	0.061 (2)	0.440 (9)
H11C	0.2014	0.3067	0.3476	0.073*	0.440 (9)
H11D	0.2934	0.2696	0.2656	0.073*	0.440 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Nb1	0.0085 (1)	0.0181 (1)	0.0207 (1)	0.00211 (8)	0.00572 (8)	0.00766 (8)
Nb2	0.0103 (1)	0.0202 (1)	0.0109 (1)	−0.00342 (8)	0.00341 (7)	0.00206 (8)
Nb3	0.0105 (1)	0.0203 (1)	0.0106 (1)	−0.00263 (8)	0.00461 (7)	0.00265 (8)
Cl1	0.0214 (3)	0.0175 (3)	0.0344 (3)	−0.0016 (2)	0.0154 (3)	−0.0019 (2)
Cl2	0.0189 (3)	0.0219 (3)	0.0337 (3)	0.0011 (2)	0.0184 (3)	0.0020 (3)
Cl3	0.0192 (3)	0.0299 (4)	0.0647 (5)	0.0131 (3)	0.0181 (3)	0.0254 (4)
Cl4	0.0140 (3)	0.0303 (3)	0.0215 (3)	−0.0005 (2)	0.0017 (2)	0.0159 (3)
Cl5	0.0271 (3)	0.0392 (4)	0.0125 (3)	−0.0172 (3)	0.0082 (2)	−0.0039 (3)
Cl6	0.0082 (3)	0.0335 (4)	0.0265 (3)	−0.0021 (2)	−0.0013 (2)	0.0150 (3)
Cl7	0.0272 (3)	0.0379 (4)	0.0182 (3)	−0.0185 (3)	0.0051 (2)	−0.0044 (3)
Cl8	0.0316 (4)	0.0476 (4)	0.0158 (3)	−0.0161 (3)	0.0139 (3)	−0.0001 (3)
Cl9	0.0112 (2)	0.0224 (3)	0.0147 (3)	−0.0039 (2)	0.0053 (2)	0.0028 (2)
S1	0.0379 (4)	0.0470 (5)	0.0320 (4)	−0.0094 (4)	0.0118 (3)	0.0157 (4)
N1	0.043 (2)	0.042 (2)	0.018 (1)	−0.026 (1)	0.013 (1)	−0.010 (1)
C1	0.032 (2)	0.042 (2)	0.017 (1)	−0.014 (1)	0.003 (1)	0.001 (1)
C2	0.047 (2)	0.046 (2)	0.020 (1)	−0.019 (2)	0.013 (1)	−0.002 (1)
C3	0.060 (2)	0.063 (3)	0.034 (2)	−0.020 (2)	0.029 (2)	−0.003 (2)
C4	0.076 (3)	0.063 (3)	0.049 (2)	−0.022 (2)	0.038 (2)	−0.025 (2)
C5	0.098 (3)	0.042 (2)	0.064 (3)	−0.034 (2)	0.051 (3)	−0.032 (2)
C6	0.089 (3)	0.041 (2)	0.055 (2)	−0.040 (2)	0.047 (2)	−0.031 (2)
C7	0.054 (2)	0.042 (2)	0.022 (1)	−0.028 (2)	0.019 (1)	−0.017 (1)
O1A	0.035 (2)	0.030 (2)	0.043 (2)	−0.010 (1)	0.020 (1)	−0.007 (1)
C8A	0.038 (2)	0.033 (2)	0.047 (2)	−0.011 (1)	0.016 (1)	−0.007 (1)
C9A	0.040 (2)	0.033 (2)	0.049 (2)	−0.010 (1)	0.015 (1)	−0.008 (1)
C10A	0.038 (2)	0.032 (2)	0.048 (2)	−0.010 (1)	0.017 (1)	−0.007 (1)
C11A	0.034 (2)	0.030 (2)	0.044 (2)	−0.010 (1)	0.021 (1)	−0.006 (1)
O1B	0.067 (3)	0.055 (3)	0.078 (4)	−0.021 (2)	0.050 (3)	−0.002 (2)
C8B	0.068 (3)	0.056 (3)	0.080 (4)	−0.022 (2)	0.049 (3)	−0.003 (2)
C9B	0.068 (3)	0.055 (3)	0.080 (4)	−0.022 (2)	0.049 (3)	−0.004 (2)
C10B	0.068 (3)	0.054 (3)	0.079 (4)	−0.021 (2)	0.050 (3)	−0.003 (2)
C11B	0.067 (3)	0.054 (3)	0.078 (4)	−0.021 (2)	0.051 (3)	−0.002 (2)

Geometric parameters (Å, º) top

Nb1—Cl6ⁱ	2.4234 (7)	C3—C4	1.363 (6)
Nb1—Cl2	2.4242 (6)	C3—H3	0.9500
Nb1—Cl1	2.4281 (7)	C4—C5	1.405 (5)
Nb1—Cl4	2.4326 (6)	C4—H4	0.9500
Nb1—Cl3	2.4774 (7)	C5—C6	1.368 (6)
Nb1—Nb2ⁱ	3.0215 (3)	C5—H5	0.9500
Nb1—Nb3	3.0216 (3)	C6—C7	1.392 (5)
Nb1—Nb3ⁱ	3.0261 (3)	C6—H6	0.9500
Nb1—Nb2	3.0342 (3)	O1A—C11A	1.452 (3)
Nb2—Cl6	2.4206 (7)	O1A—C8A	1.454 (3)
Nb2—Cl1	2.4209 (7)	C8A—C9A	1.501 (4)
Nb2—Cl9ⁱ	2.4276 (6)	C8A—H8A	0.9900
Nb2—Cl5	2.4280 (6)	C8A—H8B	0.9900
Nb2—Cl7	2.4809 (7)	C9A—C10A	1.479 (7)
Nb2—Nb1ⁱ	3.0215 (3)	C9A—H9A	0.9900
Nb2—Nb3ⁱ	3.0258 (3)	C9A—H9B	0.9900
Nb2—Nb3	3.0286 (3)	C10A—C11A	1.498 (4)
Nb3—Cl2	2.4215 (7)	C10A—H10A	0.9900
Nb3—Cl9	2.4256 (6)	C10A—H10B	0.9900
Nb3—Cl5	2.4282 (7)	C11A—H11A	0.9900
Nb3—Cl4ⁱ	2.4296 (7)	C11A—H11B	0.9900
Nb3—Cl8	2.5013 (6)	O1B—C11B	1.451 (3)
Nb3—Nb2ⁱ	3.0258 (3)	O1B—C8B	1.453 (3)
Nb3—Nb1ⁱ	3.0260 (3)	C8B—C9B	1.500 (4)
Cl4—Nb3ⁱ	2.4297 (7)	C8B—H8C	0.9900
Cl6—Nb1ⁱ	2.4234 (7)	C8B—H8D	0.9900
Cl9—Nb2ⁱ	2.4276 (6)	C9B—C10B	1.477 (7)
S1—C1	1.689 (3)	C9B—H9C	0.9900
S1—C2	1.733 (4)	C9B—H9D	0.9900
N1—C1	1.304 (4)	C10B—C11B	1.497 (4)
N1—C7	1.388 (4)	C10B—H10C	0.9900
N1—H1A	0.83 (4)	C10B—H10D	0.9900
C1—H1B	0.9500	C11B—H11C	0.9900
C2—C3	1.396 (5)	C11B—H11D	0.9900
C2—C7	1.398 (4)

Cl6ⁱ—Nb1—Cl2	88.91 (2)	Cl5—Nb3—Nb1ⁱ	94.04 (2)
Cl6ⁱ—Nb1—Cl1	167.35 (2)	Cl4ⁱ—Nb3—Nb1ⁱ	51.55 (2)
Cl2—Nb1—Cl1	89.40 (2)	Cl8—Nb3—Nb1ⁱ	134.01 (2)
Cl6ⁱ—Nb1—Cl4	90.07 (2)	Nb1—Nb3—Nb1ⁱ	90.026 (8)
Cl2—Nb1—Cl4	167.17 (2)	Nb2ⁱ—Nb3—Nb1ⁱ	60.181 (7)
Cl1—Nb1—Cl4	88.80 (2)	Cl2—Nb3—Nb2	94.40 (2)
Cl6ⁱ—Nb1—Cl3	83.84 (3)	Cl9—Nb3—Nb2	141.61 (2)
Cl2—Nb1—Cl3	84.50 (2)	Cl5—Nb3—Nb2	51.42 (2)
Cl1—Nb1—Cl3	83.52 (3)	Cl4ⁱ—Nb3—Nb2	94.38 (2)
Cl4—Nb1—Cl3	82.67 (2)	Cl8—Nb3—Nb2	135.10 (2)
Cl6ⁱ—Nb1—Nb2ⁱ	51.37 (2)	Nb1—Nb3—Nb2	60.198 (7)
Cl2—Nb1—Nb2ⁱ	94.84 (2)	Nb2ⁱ—Nb3—Nb2	90.153 (8)
Cl1—Nb1—Nb2ⁱ	141.28 (2)	Nb1ⁱ—Nb3—Nb2	59.874 (7)
Cl4—Nb1—Nb2ⁱ	94.50 (2)	Nb2—Cl1—Nb1	77.47 (2)
Cl3—Nb1—Nb2ⁱ	135.18 (2)	Nb3—Cl2—Nb1	77.15 (2)
Cl6ⁱ—Nb1—Nb3	94.00 (2)	Nb3ⁱ—Cl4—Nb1	76.98 (2)
Cl2—Nb1—Nb3	51.38 (2)	Nb2—Cl5—Nb3	77.17 (2)
Cl1—Nb1—Nb3	94.73 (2)	Nb2—Cl6—Nb1ⁱ	77.18 (2)
Cl4—Nb1—Nb3	141.44 (2)	Nb3—Cl9—Nb2ⁱ	77.14 (2)
Cl3—Nb1—Nb3	135.89 (2)	C1—S1—C2	90.9 (2)
Nb2ⁱ—Nb1—Nb3	60.092 (8)	C1—N1—C7	114.3 (3)
Cl6ⁱ—Nb1—Nb3ⁱ	95.25 (2)	C1—N1—H1A	121 (3)
Cl2—Nb1—Nb3ⁱ	141.35 (2)	C7—N1—H1A	125 (3)
Cl1—Nb1—Nb3ⁱ	93.89 (2)	N1—C1—S1	113.6 (3)
Cl4—Nb1—Nb3ⁱ	51.47 (2)	N1—C1—H1B	123.2
Cl3—Nb1—Nb3ⁱ	134.14 (2)	S1—C1—H1B	123.2
Nb2ⁱ—Nb1—Nb3ⁱ	60.105 (7)	C3—C2—C7	120.4 (3)
Nb3—Nb1—Nb3ⁱ	89.974 (8)	C3—C2—S1	129.9 (3)
Cl6ⁱ—Nb1—Nb2	141.48 (2)	C7—C2—S1	109.7 (3)
Cl2—Nb1—Nb2	94.21 (2)	C4—C3—C2	117.7 (3)
Cl1—Nb1—Nb2	51.16 (2)	C4—C3—H3	121.1
Cl4—Nb1—Nb2	94.55 (2)	C2—C3—H3	121.1
Cl3—Nb1—Nb2	134.68 (2)	C3—C4—C5	121.9 (4)
Nb2ⁱ—Nb1—Nb2	90.127 (8)	C3—C4—H4	119.1
Nb3—Nb1—Nb2	60.015 (7)	C5—C4—H4	119.1
Nb3ⁱ—Nb1—Nb2	59.906 (7)	C6—C5—C4	120.9 (4)
Cl6—Nb2—Cl1	167.24 (2)	C6—C5—H5	119.6
Cl6—Nb2—Cl9ⁱ	88.70 (2)	C4—C5—H5	119.6
Cl1—Nb2—Cl9ⁱ	88.53 (2)	C5—C6—C7	117.7 (3)
Cl6—Nb2—Cl5	89.69 (2)	C5—C6—H6	121.1
Cl1—Nb2—Cl5	90.29 (2)	C7—C6—H6	121.1
Cl9ⁱ—Nb2—Cl5	167.33 (2)	N1—C7—C6	127.3 (3)
Cl6—Nb2—Cl7	84.42 (3)	N1—C7—C2	111.5 (3)
Cl1—Nb2—Cl7	82.90 (3)	C6—C7—C2	121.3 (3)
Cl9ⁱ—Nb2—Cl7	84.05 (2)	C11A—O1A—C8A	110.3 (3)
Cl5—Nb2—Cl7	83.29 (2)	O1A—C8A—C9A	105.2 (3)
Cl6—Nb2—Nb1ⁱ	51.45 (2)	O1A—C8A—H8A	110.7
Cl1—Nb2—Nb1ⁱ	141.24 (2)	C9A—C8A—H8A	110.7
Cl9ⁱ—Nb2—Nb1ⁱ	94.66 (2)	O1A—C8A—H8B	110.7
Cl5—Nb2—Nb1ⁱ	94.15 (2)	C9A—C8A—H8B	110.7
Cl7—Nb2—Nb1ⁱ	135.86 (2)	H8A—C8A—H8B	108.8
Cl6—Nb2—Nb3ⁱ	93.95 (2)	C10A—C9A—C8A	105.3 (2)
Cl1—Nb2—Nb3ⁱ	94.05 (2)	C10A—C9A—H9A	110.7
Cl9ⁱ—Nb2—Nb3ⁱ	51.40 (2)	C8A—C9A—H9A	110.7
Cl5—Nb2—Nb3ⁱ	141.26 (2)	C10A—C9A—H9B	110.7
Cl7—Nb2—Nb3ⁱ	135.44 (2)	C8A—C9A—H9B	110.7
Nb1ⁱ—Nb2—Nb3ⁱ	59.955 (7)	H9A—C9A—H9B	108.8
Cl6—Nb2—Nb3	95.25 (2)	C9A—C10A—C11A	105.6 (2)
Cl1—Nb2—Nb3	94.71 (2)	C9A—C10A—H10A	110.6
Cl9ⁱ—Nb2—Nb3	141.25 (2)	C11A—C10A—H10A	110.6
Cl5—Nb2—Nb3	51.42 (2)	C9A—C10A—H10B	110.6
Cl7—Nb2—Nb3	134.70 (2)	C11A—C10A—H10B	110.6
Nb1ⁱ—Nb2—Nb3	60.022 (7)	H10A—C10A—H10B	108.7
Nb3ⁱ—Nb2—Nb3	89.847 (8)	O1A—C11A—C10A	105.8 (3)
Cl6—Nb2—Nb1	141.31 (2)	O1A—C11A—H11A	110.6
Cl1—Nb2—Nb1	51.37 (2)	C10A—C11A—H11A	110.6
Cl9ⁱ—Nb2—Nb1	94.32 (2)	O1A—C11A—H11B	110.6
Cl5—Nb2—Nb1	94.78 (2)	C10A—C11A—H11B	110.6
Cl7—Nb2—Nb1	134.27 (2)	H11A—C11A—H11B	108.7
Nb1ⁱ—Nb2—Nb1	89.874 (8)	C11B—O1B—C8B	110.4 (3)
Nb3ⁱ—Nb2—Nb1	59.915 (7)	O1B—C8B—C9B	105.3 (3)
Nb3—Nb2—Nb1	59.787 (7)	O1B—C8B—H8C	110.7
Cl2—Nb3—Cl9	89.86 (2)	C9B—C8B—H8C	110.7
Cl2—Nb3—Cl5	89.50 (3)	O1B—C8B—H8D	110.7
Cl9—Nb3—Cl5	166.95 (2)	C9B—C8B—H8D	110.7
Cl2—Nb3—Cl4ⁱ	166.95 (2)	H8C—C8B—H8D	108.8
Cl9—Nb3—Cl4ⁱ	89.24 (2)	C10B—C9B—C8B	105.5 (2)
Cl5—Nb3—Cl4ⁱ	88.45 (3)	C10B—C9B—H9C	110.6
Cl2—Nb3—Cl8	84.50 (2)	C8B—C9B—H9C	110.6
Cl9—Nb3—Cl8	83.27 (2)	C10B—C9B—H9D	110.6
Cl5—Nb3—Cl8	83.69 (2)	C8B—C9B—H9D	110.6
Cl4ⁱ—Nb3—Cl8	82.46 (2)	H9C—C9B—H9D	108.8
Cl2—Nb3—Nb1	51.46 (2)	C9B—C10B—C11B	105.9 (2)
Cl9—Nb3—Nb1	94.70 (2)	C9B—C10B—H10C	110.6
Cl5—Nb3—Nb1	95.09 (2)	C11B—C10B—H10C	110.6
Cl4ⁱ—Nb3—Nb1	141.58 (2)	C9B—C10B—H10D	110.6
Cl8—Nb3—Nb1	135.96 (2)	C11B—C10B—H10D	110.6
Cl2—Nb3—Nb2ⁱ	94.79 (2)	H10C—C10B—H10D	108.7
Cl9—Nb3—Nb2ⁱ	51.46 (1)	O1B—C11B—C10B	105.8 (3)
Cl5—Nb3—Nb2ⁱ	141.56 (2)	O1B—C11B—H11C	110.6
Cl4ⁱ—Nb3—Nb2ⁱ	94.82 (2)	C10B—C11B—H11C	110.6
Cl8—Nb3—Nb2ⁱ	134.73 (2)	O1B—C11B—H11D	110.6
Nb1—Nb3—Nb2ⁱ	59.953 (8)	C10B—C11B—H11D	110.6
Cl2—Nb3—Nb1ⁱ	141.48 (2)	H11C—C11B—H11D	108.7
Cl9—Nb3—Nb1ⁱ	94.57 (2)

Symmetry code: (i) −x, −y+1, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O1A	0.83 (4)	1.86 (4)	2.691 (5)	175 (4)
N1—H1A···O1B	0.83 (4)	1.75 (4)	2.573 (6)	172 (4)

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