Tetra­kis(tri­ethyl­enediamin-1-ium) dodeca-μ2-chlorido-hexakis(thio­cyanato-κN)hexa-octa­hedro-niobate

Sperlich, E.; Köckerling, M.

doi:10.1107/S241431462300398X

Tetrakis(triethylenediamin-1-ium) dodeca-μ₂-chlorido-hexakis(thiocyanato-κN)hexa-octahedro-niobate

The crystal structure of the cluster complex salt, (C₆H₁₃N₂)₄[Nb₆(NCS)₆Cl₁₂] or (H-DABCO)₄[Nb₆Cl₁₂(NCS)₆] (DABCO = triethylenediamine or 1,4-diazabicyclo[2.2.2]octane), comprises octahedral Nb₆ cluster cores, which are μ₂-coordinated by 12 chloride ligands (bridging the octahedral edges, inner ligand sphere). Furthermore, each Nb atom is N-bonded to a terminal thiocyanate ligand (outer ligand sphere). The discrete clusters carry a charge of −4, which is compensated by four monoprotonated DABCO molecules. These are arranged in rows, which are N—H

Cl and N—H

N hydrogen bonded to the anions and among each other.

Keywords: crystal structure; niobium; cluster; chloride; DABCO.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S241431462300398X/wm4186sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S241431462300398X/wm4186Isup2.hkl Contains datablock I

CCDC reference: 2260596

checkCIF report

Key indicators

Structure: I

Single-crystal X-ray study
T = 123 K
Mean (C-C) = 0.012 Å
Disorder in main residue
R factor = 0.040
wR factor = 0.093
Data-to-parameter ratio = 27.5

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  N7       ..N7       .       2.83 Ang.
                                          2/3-x,4/3-y,1/3-z  =     13_565 Check

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 =     2.003
            Value of mu given      =     1.977
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT234_ALERT_4_C Large Hirshfeld Difference N5       --C5       .       0.16 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference C5       --C6       .       0.22 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference C9       --C10      .       0.20 Ang.
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of         N4 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        Nb4 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         C4 Check
PLAT243_ALERT_4_C High   'Solvent' Ueq as Compared to Neighbors of         C5 Check
PLAT243_ALERT_4_C High   'Solvent' Ueq as Compared to Neighbors of         C9 Check
PLAT243_ALERT_4_C High   'Solvent' Ueq as Compared to Neighbors of        C11 Check
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of         N6 Check
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of         C7 Check
PLAT244_ALERT_4_C Low    'Solvent' Ueq as Compared to Neighbors of        C10 Check
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.5 Note
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0118 Ang.
PLAT420_ALERT_2_C D-H Bond Without Acceptor  N10      --H10N     .     Please Check
PLAT715_ALERT_1_C D-H     Unknown or Inconsistent Label ..........       N12A Check
                    N12A        H12N
PLAT716_ALERT_1_C H...A   Unknown or Inconsistent Label ..........       H12N Check
                    H12N        N6
PLAT717_ALERT_1_C D...A   Unknown or Inconsistent Label ..........       N12A Check
                    N12A        N6
PLAT718_ALERT_1_C D-H..A  Unknown or Inconsistent Label ..........       N12A Check
                    N12A        H12N        N6
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          3 Report
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.77Ang From Cl8             1.96 eA-3
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.69Ang From Nb4             1.86 eA-3
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.69Ang From Nb3             1.77 eA-3
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.00Ang From C6              1.75 eA-3
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.41Ang From C10             1.54 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.74Ang From Cl8            -1.77 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.69Ang From Nb4            -1.68 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H5N       .      -0.40 eA-3

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          5 Report
PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ...      0.250 Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large     223.51 Why ?
PLAT093_ALERT_1_G No s.u.'s on H-positions, Refinement Reported as      mixed Check
PLAT230_ALERT_2_G Hirshfeld Test Diff for    S2A_B    --C2       .        5.2 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Nb1      --N1       .        5.6 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Nb1      --Cl4_a    .        5.7 s.u.
PLAT300_ALERT_4_G Atom Site Occupancy of N11B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of N12B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C15B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C16B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C17B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C18B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C19B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C20B_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H11N_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H15C_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H15D_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H16C_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H16D_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H17C_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H17D_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H18C_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H18D_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H19C_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H19D_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H20C_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H20D_F     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of N11A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of N12A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C15A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C16A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C17A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C18A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C19A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of C20A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H12N_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H15A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H15B_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H16A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H16B_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H17A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H17B_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H18A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H18B_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H19A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H19B_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H20A_E     Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of H20B_E     Constrained at        0.5 Check
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )        11% Note
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  4  )      10.50 Check
PLAT480_ALERT_4_G Long H...A H-Bond Reported H10N     ..CL7      .       2.90 Ang.
PLAT480_ALERT_4_G Long H...A H-Bond Reported H10N     ..CL7      .       2.90 Ang.
PLAT480_ALERT_4_G Long H...A H-Bond Reported H10N     ..CL7      .       2.90 Ang.
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........         46 Note
PLAT802_ALERT_4_G CIF Input Record(s) with more than 80 Characters          1 Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          8 Note
PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          3 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          0 Info
PLAT982_ALERT_1_G The Cl-f'=    0.1507 Deviates from  IT-value =       0.1484 Check
PLAT982_ALERT_1_G The Nb-f'=   -2.0614 Deviates from  IT-value =      -2.0727 Check
PLAT982_ALERT_1_G The  S-f'=    0.1265 Deviates from  IT-value =       0.1246 Check
PLAT983_ALERT_1_G The Cl-f"=    0.1611 Deviates from  IT-Value =       0.1585 Check
PLAT983_ALERT_1_G The Nb-f"=    0.6336 Deviates from  IT-Value =       0.6215 Check
PLAT983_ALERT_1_G The  S-f"=    0.1256 Deviates from  IT-Value =       0.1234 Check

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

  14 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  21 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
  60 ALERT type 4 Improvement, methodology, query or suggestion
   1 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: SHELXS (Sheldrick, 2008); program(s) used to refine structure: SHELXL (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg & Putz, 2019); software used to prepare material for publication: publCIF (Westrip, 2010).

Tetrakis(triethylenediamin-1-ium) dodeca-µ₂-chlorido-hexakis(thiocyanato-κN)hexa-octahedro-niobate top

Crystal data top

(C₆H₁₃N₂)₄[Nb₆(NCS)₆Cl₁₂]	D_x = 2.092 Mg m⁻³
M_r = 1784.08	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3	Cell parameters from 9867 reflections
a = 25.399 (2) Å	θ = 2.5–32.6°
c = 30.418 (2) Å	µ = 1.98 mm⁻¹
V = 16993 (3) Å³	T = 123 K
Z = 12	Block, black
F(000) = 10512	0.30 × 0.20 × 0.20 mm

Data collection top

Bruker APEXII CCD diffractometer	11834 reflections with I > 2σ(I)
Radiation source: microfocus sealed tube	R_int = 0.040
φ and ω scans	θ_max = 32.6°, θ_min = 1.1°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −38→38
	k = −38→38
84629 measured reflections	l = −46→46
13784 independent 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)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.093	H atoms treated by a mixture of independent and constrained refinement
S = 1.09	w = 1/[σ²(F_o²) + (0.020P)² + 223.5098P] where P = (F_o² + 2F_c²)/3
13784 reflections	(Δ/σ)_max = 0.002
502 parameters	Δρ_max = 2.03 e Å⁻³
0 restraints	Δρ_min = −1.79 e Å⁻³

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.

Refinement. C-and N-bound hydrogen atoms were placed on idealized positions and refined using a riding models.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Nb1	0.15274 (2)	0.27928 (2)	0.38766 (2)	0.01794 (5)
Nb2	0.21875 (2)	0.30094 (2)	0.30483 (2)	0.01810 (5)
Nb3	0.24363 (2)	0.40316 (2)	0.36253 (2)	0.01897 (5)
Nb4	0.65963 (2)	0.39594 (2)	0.37251 (2)	0.02176 (6)
Cl1	0.20921 (4)	0.22977 (4)	0.36270 (3)	0.0306 (2)
Cl2	0.24134 (4)	0.35140 (4)	0.43131 (3)	0.0304 (2)
Cl3	0.13796 (4)	0.21431 (3)	0.26443 (3)	0.0296 (2)
Cl4	0.24550 (4)	0.35960 (4)	0.23630 (2)	0.0260 (1)
Cl5	0.31827 (3)	0.37626 (4)	0.33539 (3)	0.0296 (2)
Cl6	0.27439 (3)	0.47858 (3)	0.30297 (3)	0.0271 (1)
Cl7	0.73993 (4)	0.41477 (4)	0.42584 (2)	0.0305 (2)
Cl8	0.72998 (6)	0.48879 (4)	0.33235 (3)	0.0453 (3)
S1	0.17220 (6)	0.16375 (5)	0.50800 (4)	0.0499 (3)
S2B_a	0.3823 (2)	0.2647 (2)	0.2775 (6)	0.065 (2)	0.49 (3)
S2A_b	0.3887 (3)	0.2711 (4)	0.2966 (3)	0.049 (2)	0.51 (3)
S3A_c	0.4484 (1)	0.5661 (4)	0.3962 (4)	0.043 (1)	0.49 (3)
S3B_d	0.4442 (2)	0.5774 (2)	0.3810 (3)	0.035 (1)	0.51 (3)
S4	0.67419 (8)	0.51041 (6)	0.50030 (4)	0.0591 (4)
N1	0.1412 (1)	0.2221 (1)	0.4453 (1)	0.0304 (6)
N2	0.2775 (2)	0.2684 (1)	0.2764 (1)	0.0343 (7)
N3	0.3273 (1)	0.4780 (2)	0.3911 (1)	0.0355 (7)
N4	0.6530 (2)	0.4609 (2)	0.4167 (1)	0.0454 (9)
N5	0.4310 (4)	0.4556 (4)	0.2629 (2)	0.102 (2)
H5N	0.3886	0.4307	0.2745	0.123*
N6	0.5372 (3)	0.5180 (2)	0.2347 (1)	0.062 (1)
N7	0.3333	0.6667	0.2131 (2)	0.0427 (13)
N8	0.3333	0.6667	0.2968 (2)	0.0291 (10)
H8N	0.3333	0.6667	0.3297	0.035*
N9	0.3333	0.6667	0.3887 (2)	0.0270 (9)
N10	0.3333	0.6667	0.4714 (2)	0.0450 (14)
H10N	0.3333	0.6667	0.5043	0.054*
C1	0.1537 (2)	0.1978 (2)	0.4716 (1)	0.0248 (6)
C2	0.3228 (2)	0.2677 (2)	0.2819 (2)	0.045 (1)
C3	0.3772 (2)	0.5172 (2)	0.3901 (1)	0.0341 (7)
C4	0.6618 (2)	0.4819 (2)	0.4516 (1)	0.0365 (8)
C5	0.4472 (5)	0.5205 (5)	0.2635 (3)	0.126 (4)
H5A	0.4258	0.5292	0.2399	0.151*
H5B	0.4370	0.5316	0.2922	0.151*
C6	0.5137 (5)	0.5538 (4)	0.2561 (3)	0.111 (4)
H6A	0.5243	0.5900	0.2378	0.133*
H6B	0.5344	0.5684	0.2848	0.133*
C7	0.4319 (3)	0.4367 (3)	0.2174 (2)	0.066 (2)
H7A	0.3981	0.4355	0.2003	0.079*
H7B	0.4277	0.3958	0.2167	0.079*
C8	0.4923 (3)	0.4833 (3)	0.1985 (2)	0.068 (2)
H8A	0.4867	0.5121	0.1798	0.082*
H8B	0.5085	0.4628	0.1798	0.082*
C9	0.4715 (4)	0.4440 (6)	0.2907 (3)	0.139 (5)
H9A	0.4543	0.3998	0.2953	0.166*
H9B	0.4772	0.4638	0.3197	0.166*
C10	0.5314 (4)	0.4705 (3)	0.2665 (2)	0.080 (2)
H10A	0.5654	0.4887	0.2879	0.097*
H10B	0.5338	0.4378	0.2505	0.097*
C11	0.3838 (3)	0.6592 (3)	0.2300 (2)	0.062 (1)
H11A	0.4232	0.6961	0.2235	0.074*
H11B	0.3834	0.6242	0.2154	0.074*
C12	0.3769 (2)	0.6486 (2)	0.2798 (2)	0.0367 (8)
H12A	0.3618	0.6051	0.2863	0.044*
H12B	0.4169	0.6729	0.2944	0.044*
C13	0.3955 (2)	0.6873 (2)	0.4054 (1)	0.0384 (8)
H13A	0.4221	0.7312	0.3992	0.046*
H13B	0.4128	0.6647	0.3904	0.046*
C14	0.3926 (2)	0.6760 (3)	0.4550 (2)	0.050 (1)
H14A	0.3961	0.6396	0.4612	0.060*
H14B	0.4265	0.7114	0.4699	0.060*
N11A_e	0.4625 (7)	0.4273 (5)	0.4797 (5)	0.057 (3)	0.5
N12A_e	0.4077 (5)	0.3171 (4)	0.4549 (4)	0.035 (2)	0.5
H12N_e	0.3860	0.2738	0.4449	0.042*	0.5
C15A_e	0.4859 (5)	0.3932 (5)	0.5062 (4)	0.054 (2)	0.5
H15A_e	0.4796	0.3967	0.5379	0.065*	0.5
H15B_e	0.5299	0.4104	0.5009	0.065*	0.5
C16A_e	0.4508 (4)	0.3260 (5)	0.4919 (3)	0.045 (2)	0.5
H16A_e	0.4800	0.3132	0.4823	0.054*	0.5
H16B_e	0.4277	0.3004	0.5173	0.054*	0.5
C17A_e	0.4761 (7)	0.4240 (5)	0.4331 (3)	0.065 (3)	0.5
H17A_e	0.5206	0.4429	0.4290	0.078*	0.5
H17B_e	0.4617	0.4468	0.4151	0.078*	0.5
C18A_e	0.4454 (5)	0.3588 (5)	0.4180 (3)	0.055 (3)	0.5
H18A_e	0.4764	0.3485	0.4086	0.066*	0.5
H18B_e	0.4189	0.3533	0.3925	0.066*	0.5
C19A_e	0.3974 (5)	0.4013 (6)	0.4859 (4)	0.060 (3)	0.5
H19A_e	0.3831	0.4251	0.4691	0.072*	0.5
H19B_e	0.3885	0.4030	0.5174	0.072*	0.5
C20A_e	0.3641 (5)	0.3353 (5)	0.4703 (4)	0.052 (2)	0.5
H20A_e	0.3397	0.3084	0.4947	0.062*	0.5
H20B_e	0.3361	0.3306	0.4460	0.062*	0.5
N11B_f	0.5240 (5)	0.5477 (5)	0.5162 (4)	0.047 (2)	0.5
H11N_f	0.5007	0.5040	0.5071	0.08 (4)*	0.5
N12B_f	0.5836 (6)	0.6587 (5)	0.5401 (4)	0.046 (2)	0.5
C15B_f	0.5711 (5)	0.5853 (5)	0.4820 (3)	0.053 (2)	0.5
H15C_f	0.5508	0.5875	0.4548	0.064*	0.5
H15D_f	0.5959	0.5664	0.4747	0.064*	0.5
C16B_f	0.6117 (6)	0.6492 (6)	0.5005 (4)	0.066 (3)	0.5
H16C_f	0.6520	0.6546	0.5082	0.079*	0.5
H16D_f	0.6178	0.6799	0.4780	0.079*	0.5
C17B_f	0.4833 (5)	0.5719 (6)	0.5220 (4)	0.065 (3)	0.5
H17C_f	0.4556	0.5515	0.5471	0.078*	0.5
H17D_f	0.4583	0.5644	0.4953	0.078*	0.5
C18B_f	0.5214 (6)	0.6400 (6)	0.5307 (6)	0.078 (4)	0.5
H18C_f	0.5196	0.6624	0.5046	0.094*	0.5
H18D_f	0.5039	0.6507	0.5559	0.094*	0.5
C19B_f	0.5587 (6)	0.5548 (6)	0.5587 (3)	0.064 (3)	0.5
H19C_f	0.5310	0.5260	0.5811	0.077*	0.5
H19D_f	0.5917	0.5456	0.5533	0.077*	0.5
C20B_f	0.5852 (7)	0.6194 (7)	0.5751 (4)	0.071 (3)	0.5
H20C_f	0.5617	0.6201	0.6008	0.085*	0.5
H20D_f	0.6278	0.6349	0.5846	0.085*	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Nb1	0.0177 (1)	0.0180 (1)	0.0190 (1)	0.00960 (9)	0.00115 (8)	0.00467 (8)
Nb2	0.0173 (1)	0.0171 (1)	0.0219 (1)	0.01010 (9)	0.00278 (8)	0.00274 (8)
Nb3	0.0150 (1)	0.0168 (1)	0.0208 (1)	0.00477 (8)	−0.00174 (8)	−0.00031 (8)
Nb4	0.0344 (1)	0.0229 (1)	0.0134 (1)	0.0183 (1)	−0.00046 (9)	−0.00156 (8)
Cl1	0.0358 (4)	0.0326 (4)	0.0356 (4)	0.0263 (3)	0.0092 (3)	0.0136 (3)
Cl2	0.0268 (3)	0.0362 (4)	0.0221 (3)	0.0111 (3)	−0.0070 (3)	0.0030 (3)
Cl3	0.0323 (4)	0.0202 (3)	0.0319 (4)	0.0097 (3)	0.0030 (3)	−0.0067 (3)
Cl4	0.0296 (3)	0.0275 (3)	0.0239 (3)	0.0165 (3)	0.0086 (3)	0.0068 (3)
Cl5	0.0156 (3)	0.0345 (4)	0.0377 (4)	0.0118 (3)	0.0001 (3)	0.0010 (3)
Cl6	0.0251 (3)	0.0165 (3)	0.0326 (4)	0.0051 (2)	0.0029 (3)	0.0053 (3)
Cl7	0.0320 (4)	0.0323 (4)	0.0178 (3)	0.0089 (3)	−0.0054 (3)	−0.0070 (3)
Cl8	0.0811 (8)	0.0182 (3)	0.0238 (4)	0.0152 (4)	0.0029 (4)	−0.0004 (3)
S1	0.0696 (8)	0.0401 (5)	0.0467 (6)	0.0325 (5)	−0.0303 (5)	−0.0006 (4)
S2B_a	0.041 (1)	0.091 (2)	0.082 (7)	0.047 (2)	−0.016 (2)	−0.036 (2)
S2A_b	0.036 (2)	0.082 (3)	0.041 (3)	0.041 (2)	0.000 (1)	−0.006 (2)
S3A_c	0.0190 (9)	0.039 (2)	0.053 (3)	0.0002 (9)	−0.005 (1)	0.005 (2)
S3B_d	0.0195 (8)	0.028 (1)	0.047 (3)	0.0042 (8)	0.002 (1)	0.001 (1)
S4	0.093 (1)	0.0522 (7)	0.0262 (5)	0.0316 (7)	−0.0004 (5)	−0.0151 (4)
N1	0.032 (1)	0.033 (1)	0.030 (1)	0.019 (1)	0.006 (1)	0.012 (1)
N2	0.036 (2)	0.032 (1)	0.045 (2)	0.024 (1)	0.016 (1)	0.009 (1)
N3	0.025 (1)	0.032 (2)	0.033 (2)	0.002 (1)	−0.004 (1)	−0.007 (1)
N4	0.088 (3)	0.044 (2)	0.026 (1)	0.049 (2)	−0.003 (2)	−0.006 (1)
N5	0.117 (5)	0.174 (8)	0.042 (3)	0.093 (6)	0.016 (3)	0.030 (4)
N6	0.114 (4)	0.063 (3)	0.033 (2)	0.061 (3)	−0.012 (2)	−0.002 (2)
N7	0.042 (2)	0.042 (2)	0.044 (3)	0.021 (1)	0.00	0.00
N8	0.024 (1)	0.024 (1)	0.040 (3)	0.0118 (6)	0.00	0.00
N9	0.027 (1)	0.027 (1)	0.028 (2)	0.0133 (7)	0.00	0.00
N10	0.051 (2)	0.051 (2)	0.032 (3)	0.026 (1)	0.00	0.00
C1	0.026 (1)	0.026 (1)	0.024 (1)	0.015 (1)	−0.001 (1)	0.001 (1)
C2	0.039 (2)	0.038 (2)	0.067 (3)	0.026 (2)	0.026 (2)	0.015 (2)
C3	0.022 (1)	0.030 (2)	0.043 (2)	0.008 (1)	−0.001 (1)	−0.013 (1)
C4	0.061 (2)	0.025 (2)	0.025 (2)	0.023 (2)	0.005 (2)	0.001 (1)
C5	0.146 (9)	0.17 (1)	0.123 (8)	0.122 (9)	−0.045 (7)	−0.086 (7)
C6	0.19 (1)	0.080 (5)	0.098 (6)	0.099 (7)	−0.065 (6)	−0.047 (4)
C7	0.088 (4)	0.057 (3)	0.058 (3)	0.040 (3)	0.007 (3)	0.001 (3)
C8	0.101 (5)	0.067 (4)	0.040 (3)	0.045 (4)	−0.010 (3)	−0.010 (2)
C9	0.114 (7)	0.25 (1)	0.071 (5)	0.107 (9)	0.015 (5)	0.085 (7)
C10	0.125 (6)	0.062 (4)	0.061 (4)	0.051 (4)	−0.025 (4)	0.007 (3)
C11	0.063 (3)	0.084 (4)	0.060 (3)	0.053 (3)	−0.001 (3)	−0.013 (3)
C12	0.028 (2)	0.032 (2)	0.057 (2)	0.020 (1)	−0.002 (2)	−0.003 (2)
C13	0.026 (2)	0.042 (2)	0.046 (2)	0.015 (2)	−0.002 (2)	−0.002 (2)
C14	0.043 (2)	0.063 (3)	0.043 (2)	0.025 (2)	−0.014 (2)	−0.010 (2)
N11A_e	0.069 (8)	0.038 (5)	0.053 (6)	0.019 (6)	0.014 (5)	0.013 (5)
N12A_e	0.041 (4)	0.038 (4)	0.034 (4)	0.025 (4)	0.012 (3)	0.013 (4)
C15A_e	0.046 (5)	0.059 (6)	0.056 (6)	0.025 (5)	0.013 (4)	0.019 (5)
C16A_e	0.050 (5)	0.065 (6)	0.036 (4)	0.042 (5)	0.011 (4)	0.020 (4)
C17A_e	0.10 (1)	0.065 (7)	0.041 (5)	0.052 (7)	0.024 (6)	0.023 (5)
C18A_e	0.066 (6)	0.070 (7)	0.039 (4)	0.041 (6)	0.020 (4)	0.020 (4)
C19A_e	0.063 (6)	0.074 (7)	0.064 (7)	0.051 (6)	0.009 (5)	−0.001 (6)
C20A_e	0.055 (6)	0.060 (6)	0.060 (6)	0.043 (5)	0.015 (5)	0.010 (5)
N11B_f	0.048 (6)	0.043 (5)	0.043 (5)	0.018 (5)	0.013 (4)	0.012 (5)
N12B_f	0.047 (5)	0.057 (6)	0.043 (5)	0.032 (6)	0.000 (4)	0.001 (5)
C15B_f	0.070 (7)	0.068 (6)	0.035 (4)	0.046 (6)	0.014 (4)	0.012 (4)
C16B_f	0.069 (7)	0.065 (7)	0.053 (6)	0.025 (6)	0.030 (6)	0.010 (5)
C17B_f	0.048 (6)	0.093 (9)	0.060 (6)	0.040 (6)	0.009 (5)	0.021 (6)
C18B_f	0.060 (7)	0.082 (9)	0.12 (1)	0.060 (7)	−0.014 (8)	−0.013 (9)
C19B_f	0.089 (8)	0.099 (9)	0.040 (5)	0.072 (8)	0.021 (5)	0.031 (5)
C20B_f	0.081 (9)	0.10 (1)	0.044 (5)	0.060 (8)	−0.007 (5)	0.009 (6)

Geometric parameters (Å, º) top

Nb1—N1	2.200 (3)	C5—C6	1.48 (1)
Nb1—Cl1	2.4530 (8)	C5—H5A	0.9900
Nb1—Cl6ⁱ	2.4605 (8)	C5—H5B	0.9900
Nb1—Cl2	2.4617 (8)	C6—H6A	0.9900
Nb1—Cl4ⁱ	2.4631 (8)	C6—H6B	0.9900
Nb1—Nb2ⁱ	2.9165 (4)	C7—C8	1.506 (9)
Nb1—Nb3ⁱ	2.9220 (4)	C7—H7A	0.9900
Nb1—Nb2	2.9221 (4)	C7—H7B	0.9900
Nb1—Nb3	2.9241 (4)	C8—H8A	0.9900
Nb2—N2	2.211 (3)	C8—H8B	0.9900
Nb2—Cl1	2.4467 (8)	C9—C10	1.51 (1)
Nb2—Cl4	2.4527 (8)	C9—H9A	0.9900
Nb2—Cl3	2.4593 (8)	C9—H9B	0.9900
Nb2—Cl5	2.4651 (8)	C10—H10A	0.9900
Nb2—Nb1ⁱ	2.9164 (4)	C10—H10B	0.9900
Nb2—Nb3ⁱ	2.9207 (4)	C11—C12	1.534 (7)
Nb2—Nb3	2.9293 (4)	C11—H11A	0.9900
Nb3—N3	2.201 (3)	C11—H11B	0.9900
Nb3—Cl2	2.4561 (8)	C12—H12A	0.9900
Nb3—Cl5	2.4573 (8)	C12—H12B	0.9900
Nb3—Cl3ⁱ	2.4602 (8)	C13—C14	1.532 (6)
Nb3—Cl6	2.4627 (8)	C13—H13A	0.9900
Nb3—Nb2ⁱ	2.9207 (4)	C13—H13B	0.9900
Nb3—Nb1ⁱ	2.9221 (4)	C14—H14A	0.9900
Nb4—N4	2.199 (3)	C14—H14B	0.9900
Nb4—Cl8	2.456 (1)	N11A_e—C19A_e	1.45 (2)
Nb4—Cl7ⁱⁱ	2.4568 (9)	N11A_e—C17A_e	1.47 (2)
Nb4—Cl7	2.4587 (9)	N11A_e—C15A_e	1.50 (2)
Nb4—Cl8ⁱⁱⁱ	2.462 (1)	N12A_e—C20A_e	1.47 (1)
Nb4—Nb4ⁱⁱⁱ	2.9199 (5)	N12A_e—C16A_e	1.51 (2)
Nb4—Nb4^iv	2.9199 (5)	N12A_e—C18A_e	1.51 (1)
Nb4—Nb4ⁱⁱ	2.9213 (5)	N12A_e—H12N_e	1.0000
Nb4—Nb4^v	2.9214 (5)	C15A_e—C16A_e	1.54 (2)
Cl3—Nb3ⁱ	2.4602 (8)	C15A_e—H15A_e	0.9900
Cl4—Nb1ⁱ	2.4629 (8)	C15A_e—H15B_e	0.9900
Cl6—Nb1ⁱ	2.4606 (8)	C16A_e—H16A_e	0.9900
Cl7—Nb4^v	2.4569 (9)	C16A_e—H16B_e	0.9900
Cl8—Nb4^iv	2.462 (1)	C17A_e—C18A_e	1.50 (2)
S1—C1	1.612 (3)	C17A_e—H17A_e	0.9900
S2B_a—C2	1.557 (5)	C17A_e—H17B_e	0.9900
S2A_b—C2	1.692 (7)	C18A_e—H18A_e	0.9900
S3A_c—C3	1.613 (4)	C18A_e—H18B_e	0.9900
S3B_d—C3	1.646 (5)	C19A_e—C20A_e	1.53 (2)
S4—C4	1.611 (4)	C19A_e—H19A_e	0.9900
N1—C1	1.149 (4)	C19A_e—H19B_e	0.9900
N2—C2	1.171 (5)	C20A_e—H20A_e	0.9900
N3—C3	1.156 (4)	C20A_e—H20B_e	0.9900
N4—C4	1.158 (5)	N11B_f—C17B_f	1.45 (2)
N5—C7	1.471 (8)	N11B_f—C15B_f	1.51 (1)
N5—C9	1.472 (9)	N11B_f—C19B_f	1.52 (2)
N5—C5	1.49 (1)	N11B_f—H11N_f	1.0000
N5—H5N	1.0000	N12B_f—C18B_f	1.43 (2)
N6—C6	1.466 (9)	N12B_f—C20B_f	1.48 (2)
N6—C10	1.495 (7)	N12B_f—C16B_f	1.48 (2)
N6—C8	1.512 (7)	C15B_f—C16B_f	1.53 (2)
N7—C11	1.479 (6)	C15B_f—H15C_f	0.9900
N7—C11^vi	1.479 (6)	C15B_f—H15D_f	0.9900
N7—C11^vii	1.480 (6)	C16B_f—H16C_f	0.9900
N8—C12^vii	1.488 (4)	C16B_f—H16D_f	0.9900
N8—C12^vi	1.488 (4)	C17B_f—C18B_f	1.52 (2)
N8—C12	1.489 (4)	C17B_f—H17C_f	0.9900
N8—H8N	1.0000	C17B_f—H17D_f	0.9900
N9—C13	1.483 (4)	C18B_f—H18C_f	0.9900
N9—C13^vii	1.483 (4)	C18B_f—H18D_f	0.9900
N9—C13^vi	1.483 (4)	C19B_f—C20B_f	1.51 (2)
N10—C14	1.489 (5)	C19B_f—H19C_f	0.9900
N10—C14^vii	1.489 (5)	C19B_f—H19D_f	0.9900
N10—C14^vi	1.489 (5)	C20B_f—H20C_f	0.9900
N10—H10N	1.0000	C20B_f—H20D_f	0.9900

N1—Nb1—Cl1	80.10 (8)	C12^vi—N8—C12	108.6 (3)
N1—Nb1—Cl6ⁱ	82.43 (9)	C12^vii—N8—H8N	110.3
Cl1—Nb1—Cl6ⁱ	87.98 (3)	C12^vi—N8—H8N	110.3
N1—Nb1—Cl2	80.31 (9)	C12—N8—H8N	110.3
Cl1—Nb1—Cl2	89.84 (3)	C13—N9—C13^vii	109.0 (3)
Cl6ⁱ—Nb1—Cl2	162.72 (3)	C13—N9—C13^vi	109.0 (3)
N1—Nb1—Cl4ⁱ	83.16 (8)	C13^vii—N9—C13^vi	109.0 (3)
Cl1—Nb1—Cl4ⁱ	163.08 (3)	C14—N10—C14^vii	109.3 (3)
Cl6ⁱ—Nb1—Cl4ⁱ	87.38 (3)	C14—N10—C14^vi	109.3 (3)
Cl2—Nb1—Cl4ⁱ	89.77 (3)	C14^vii—N10—C14^vi	109.3 (3)
N1—Nb1—Nb2ⁱ	136.57 (8)	C14—N10—H10N	109.6
Cl1—Nb1—Nb2ⁱ	143.33 (2)	C14^vii—N10—H10N	109.6
Cl6ⁱ—Nb1—Nb2ⁱ	95.69 (2)	C14^vi—N10—H10N	109.6
Cl2—Nb1—Nb2ⁱ	96.27 (2)	N1—C1—S1	179.1 (3)
Cl4ⁱ—Nb1—Nb2ⁱ	53.44 (2)	N2—C2—S2B_a	166.7 (8)
N1—Nb1—Nb3ⁱ	136.00 (9)	N2—C2—S2A_b	172.2 (6)
Cl1—Nb1—Nb3ⁱ	94.66 (2)	N3—C3—S3A_c	169.8 (7)
Cl6ⁱ—Nb1—Nb3ⁱ	53.63 (2)	N3—C3—S3B_d	169.7 (6)
Cl2—Nb1—Nb3ⁱ	143.65 (2)	N4—C4—S4	179.2 (4)
Cl4ⁱ—Nb1—Nb3ⁱ	95.66 (2)	C6—C5—N5	103.6 (7)
Nb2ⁱ—Nb1—Nb3ⁱ	60.229 (9)	C6—C5—H5A	111.0
N1—Nb1—Nb2	133.33 (8)	N5—C5—H5A	111.0
Cl1—Nb1—Nb2	53.29 (2)	C6—C5—H5B	111.0
Cl6ⁱ—Nb1—Nb2	96.66 (2)	N5—C5—H5B	111.0
Cl2—Nb1—Nb2	95.74 (2)	H5A—C5—H5B	109.0
Cl4ⁱ—Nb1—Nb2	143.51 (2)	N6—C6—C5	114.6 (6)
Nb2ⁱ—Nb1—Nb2	90.08 (1)	N6—C6—H6A	108.6
Nb3ⁱ—Nb1—Nb2	59.97 (1)	C5—C6—H6A	108.6
N1—Nb1—Nb3	133.73 (9)	N6—C6—H6B	108.6
Cl1—Nb1—Nb3	96.97 (2)	C5—C6—H6B	108.6
Cl6ⁱ—Nb1—Nb3	143.84 (2)	H6A—C6—H6B	107.6
Cl2—Nb1—Nb3	53.43 (2)	N5—C7—C8	106.2 (6)
Cl4ⁱ—Nb1—Nb3	96.37 (2)	N5—C7—H7A	110.5
Nb2ⁱ—Nb1—Nb3	60.009 (8)	C8—C7—H7A	110.5
Nb3ⁱ—Nb1—Nb3	90.22 (1)	N5—C7—H7B	110.5
Nb2—Nb1—Nb3	60.140 (9)	C8—C7—H7B	110.5
N2—Nb2—Cl1	80.88 (9)	H7A—C7—H7B	108.7
N2—Nb2—Cl4	82.00 (9)	C7—C8—N6	110.8 (5)
Cl1—Nb2—Cl4	162.82 (3)	C7—C8—H8A	109.5
N2—Nb2—Cl3	83.5 (1)	N6—C8—H8A	109.5
Cl1—Nb2—Cl3	88.20 (3)	C7—C8—H8B	109.5
Cl4—Nb2—Cl3	88.42 (3)	N6—C8—H8B	109.5
N2—Nb2—Cl5	79.4 (1)	H8A—C8—H8B	108.1
Cl1—Nb2—Cl5	89.22 (3)	N5—C9—C10	106.3 (6)
Cl4—Nb2—Cl5	89.08 (3)	N5—C9—H9A	110.5
Cl3—Nb2—Cl5	162.92 (3)	C10—C9—H9A	110.5
N2—Nb2—Nb1ⁱ	135.74 (8)	N5—C9—H9B	110.5
Cl1—Nb2—Nb1ⁱ	143.38 (2)	C10—C9—H9B	110.5
Cl4—Nb2—Nb1ⁱ	53.77 (2)	H9A—C9—H9B	108.7
Cl3—Nb2—Nb1ⁱ	95.52 (2)	N6—C10—C9	110.2 (6)
Cl5—Nb2—Nb1ⁱ	96.61 (2)	N6—C10—H10A	109.6
N2—Nb2—Nb3ⁱ	137.10 (9)	C9—C10—H10A	109.6
Cl1—Nb2—Nb3ⁱ	94.83 (2)	N6—C10—H10B	109.6
Cl4—Nb2—Nb3ⁱ	96.68 (2)	C9—C10—H10B	109.6
Cl3—Nb2—Nb3ⁱ	53.59 (2)	H10A—C10—H10B	108.1
Cl5—Nb2—Nb3ⁱ	143.48 (2)	N7—C11—C12	109.6 (4)
Nb1ⁱ—Nb2—Nb3ⁱ	60.125 (8)	N7—C11—H11A	109.7
N2—Nb2—Nb1	134.24 (8)	C12—C11—H11A	109.7
Cl1—Nb2—Nb1	53.49 (2)	N7—C11—H11B	109.7
Cl4—Nb2—Nb1	143.69 (2)	C12—C11—H11B	109.7
Cl3—Nb2—Nb1	96.83 (2)	H11A—C11—H11B	108.2
Cl5—Nb2—Nb1	95.17 (2)	N8—C12—C11	109.0 (4)
Nb1ⁱ—Nb2—Nb1	89.93 (1)	N8—C12—H12A	109.9
Nb3ⁱ—Nb2—Nb1	60.014 (9)	C11—C12—H12A	109.9
N2—Nb2—Nb3	132.7 (1)	N8—C12—H12B	109.9
Cl1—Nb2—Nb3	96.98 (2)	C11—C12—H12B	109.9
Cl4—Nb2—Nb3	95.70 (2)	H12A—C12—H12B	108.3
Cl3—Nb2—Nb3	143.72 (2)	N9—C13—C14	109.1 (4)
Cl5—Nb2—Nb3	53.36 (2)	N9—C13—H13A	109.9
Nb1ⁱ—Nb2—Nb3	59.983 (9)	C14—C13—H13A	109.9
Nb3ⁱ—Nb2—Nb3	90.147 (9)	N9—C13—H13B	109.9
Nb1—Nb2—Nb3	59.963 (9)	C14—C13—H13B	109.9
N3—Nb3—Cl2	83.07 (9)	H13A—C13—H13B	108.3
N3—Nb3—Cl5	80.0 (1)	N10—C14—C13	108.1 (4)
Cl2—Nb3—Cl5	87.27 (3)	N10—C14—H14A	110.1
N3—Nb3—Cl3ⁱ	83.1 (1)	C13—C14—H14A	110.1
Cl2—Nb3—Cl3ⁱ	88.24 (3)	N10—C14—H14B	110.1
Cl5—Nb3—Cl3ⁱ	162.87 (3)	C13—C14—H14B	110.1
N3—Nb3—Cl6	79.96 (9)	H14A—C14—H14B	108.4
Cl2—Nb3—Cl6	163.01 (3)	C19A_e—N11A_e—C17A_e	110 (1)
Cl5—Nb3—Cl6	88.87 (3)	C19A_e—N11A_e—C15A_e	110.9 (9)
Cl3ⁱ—Nb3—Cl6	90.63 (3)	C17A_e—N11A_e—C15A_e	108 (1)
N3—Nb3—Nb2ⁱ	136.56 (9)	C20A_e—N12A_e—C16A_e	108.6 (9)
Cl2—Nb3—Nb2ⁱ	96.29 (2)	C20A_e—N12A_e—C18A_e	109.1 (8)
Cl5—Nb3—Nb2ⁱ	143.44 (2)	C16A_e—N12A_e—C18A_e	107.0 (9)
Cl3ⁱ—Nb3—Nb2ⁱ	53.56 (2)	C20A_e—N12A_e—H12N_e	110.7
Cl6—Nb3—Nb2ⁱ	96.65 (2)	C16A_e—N12A_e—H12N_e	110.7
N3—Nb3—Nb1ⁱ	133.51 (9)	C18A_e—N12A_e—H12N_e	110.7
Cl2—Nb3—Nb1ⁱ	143.38 (2)	N11A_e—C15A_e—C16A_e	108.2 (9)
Cl5—Nb3—Nb1ⁱ	96.64 (2)	N11A_e—C15A_e—H15A_e	110.1
Cl3ⁱ—Nb3—Nb1ⁱ	96.81 (2)	C16A_e—C15A_e—H15A_e	110.1
Cl6—Nb3—Nb1ⁱ	53.56 (2)	N11A_e—C15A_e—H15B_e	110.1
Nb2ⁱ—Nb3—Nb1ⁱ	60.019 (9)	C16A_e—C15A_e—H15B_e	110.1
N3—Nb3—Nb1	136.67 (9)	H15A_e—C15A_e—H15B_e	108.4
Cl2—Nb3—Nb1	53.60 (2)	N12A_e—C16A_e—C15A_e	110.5 (7)
Cl5—Nb3—Nb1	95.30 (2)	N12A_e—C16A_e—H16A_e	109.5
Cl3ⁱ—Nb3—Nb1	95.31 (2)	C15A_e—C16A_e—H16A_e	109.5
Cl6—Nb3—Nb1	143.32 (2)	N12A_e—C16A_e—H16B_e	109.5
Nb2ⁱ—Nb3—Nb1	59.867 (8)	C15A_e—C16A_e—H16B_e	109.5
Nb1ⁱ—Nb3—Nb1	89.78 (1)	H16A_e—C16A_e—H16B_e	108.1
N3—Nb3—Nb2	133.54 (9)	N11A_e—C17A_e—C18A_e	110.4 (9)
Cl2—Nb3—Nb2	95.68 (2)	N11A_e—C17A_e—H17A_e	109.6
Cl5—Nb3—Nb2	53.60 (2)	C18A_e—C17A_e—H17A_e	109.6
Cl3ⁱ—Nb3—Nb2	143.40 (2)	N11A_e—C17A_e—H17B_e	109.6
Cl6—Nb3—Nb2	95.31 (2)	C18A_e—C17A_e—H17B_e	109.6
Nb2ⁱ—Nb3—Nb2	89.855 (9)	H17A_e—C17A_e—H17B_e	108.1
Nb1ⁱ—Nb3—Nb2	59.790 (9)	C17A_e—C18A_e—N12A_e	110.1 (8)
Nb1—Nb3—Nb2	59.898 (9)	C17A_e—C18A_e—H18A_e	109.6
N4—Nb4—Cl8	82.8 (1)	N12A_e—C18A_e—H18A_e	109.6
N4—Nb4—Cl7ⁱⁱ	80.0 (1)	C17A_e—C18A_e—H18B_e	109.6
Cl8—Nb4—Cl7ⁱⁱ	162.74 (3)	N12A_e—C18A_e—H18B_e	109.6
N4—Nb4—Cl7	79.5 (1)	H18A_e—C18A_e—H18B_e	108.2
Cl8—Nb4—Cl7	90.39 (4)	N11A_e—C19A_e—C20A_e	109.7 (8)
Cl7ⁱⁱ—Nb4—Cl7	88.07 (4)	N11A_e—C19A_e—H19A_e	109.7
N4—Nb4—Cl8ⁱⁱⁱ	83.4 (1)	C20A_e—C19A_e—H19A_e	109.7
Cl8—Nb4—Cl8ⁱⁱⁱ	88.75 (1)	N11A_e—C19A_e—H19B_e	109.7
Cl7ⁱⁱ—Nb4—Cl8ⁱⁱⁱ	87.71 (4)	C20A_e—C19A_e—H19B_e	109.7
Cl7—Nb4—Cl8ⁱⁱⁱ	162.93 (3)	H19A_e—C19A_e—H19B_e	108.2
N4—Nb4—Nb4ⁱⁱⁱ	136.9 (1)	N12A_e—C20A_e—C19A_e	110.7 (9)
Cl8—Nb4—Nb4ⁱⁱⁱ	95.17 (3)	N12A_e—C20A_e—H20A_e	109.5
Cl7ⁱⁱ—Nb4—Nb4ⁱⁱⁱ	96.27 (2)	C19A_e—C20A_e—H20A_e	109.5
Cl7—Nb4—Nb4ⁱⁱⁱ	143.51 (2)	N12A_e—C20A_e—H20B_e	109.5
Cl8ⁱⁱⁱ—Nb4—Nb4ⁱⁱⁱ	53.49 (2)	C19A_e—C20A_e—H20B_e	109.5
N4—Nb4—Nb4^iv	136.4 (1)	H20A_e—C20A_e—H20B_e	108.1
Cl8—Nb4—Nb4^iv	53.67 (2)	C17B_f—N11B_f—C15B_f	108.8 (9)
Cl7ⁱⁱ—Nb4—Nb4^iv	143.57 (2)	C17B_f—N11B_f—C19B_f	110 (1)
Cl7—Nb4—Nb4^iv	96.22 (2)	C15B_f—N11B_f—C19B_f	106 (1)
Cl8ⁱⁱⁱ—Nb4—Nb4^iv	96.98 (3)	C17B_f—N11B_f—H11N_f	110.6
Nb4ⁱⁱⁱ—Nb4—Nb4^iv	60.03 (1)	C15B_f—N11B_f—H11N_f	110.6
N4—Nb4—Nb4ⁱⁱ	133.5 (1)	C19B_f—N11B_f—H11N_f	110.6
Cl8—Nb4—Nb4ⁱⁱ	143.64 (2)	C18B_f—N12B_f—C20B_f	109 (1)
Cl7ⁱⁱ—Nb4—Nb4ⁱⁱ	53.57 (2)	C18B_f—N12B_f—C16B_f	109 (1)
Cl7—Nb4—Nb4ⁱⁱ	95.77 (2)	C20B_f—N12B_f—C16B_f	107 (1)
Cl8ⁱⁱⁱ—Nb4—Nb4ⁱⁱ	95.01 (3)	N11B_f—C15B_f—C16B_f	108.4 (8)
Nb4ⁱⁱⁱ—Nb4—Nb4ⁱⁱ	59.987 (6)	N11B_f—C15B_f—H15C_f	110.0
Nb4^iv—Nb4—Nb4ⁱⁱ	90.0	C16B_f—C15B_f—H15C_f	110.0
N4—Nb4—Nb4^v	133.0 (1)	N11B_f—C15B_f—H15D_f	110.0
Cl8—Nb4—Nb4^v	97.08 (3)	C16B_f—C15B_f—H15D_f	110.0
Cl7ⁱⁱ—Nb4—Nb4^v	95.81 (2)	H15C_f—C15B_f—H15D_f	108.4
Cl7—Nb4—Nb4^v	53.51 (2)	N12B_f—C16B_f—C15B_f	110.4 (9)
Cl8ⁱⁱⁱ—Nb4—Nb4^v	143.46 (2)	N12B_f—C16B_f—H16C_f	109.6
Nb4ⁱⁱⁱ—Nb4—Nb4^v	90.0	C15B_f—C16B_f—H16C_f	109.6
Nb4^iv—Nb4—Nb4^v	59.986 (6)	N12B_f—C16B_f—H16D_f	109.6
Nb4ⁱⁱ—Nb4—Nb4^v	60.0	C15B_f—C16B_f—H16D_f	109.6
Nb2—Cl1—Nb1	73.22 (2)	H16C_f—C16B_f—H16D_f	108.1
Nb3—Cl2—Nb1	72.97 (2)	N11B_f—C17B_f—C18B_f	108.6 (9)
Nb2—Cl3—Nb3ⁱ	72.84 (2)	N11B_f—C17B_f—H17C_f	110.0
Nb2—Cl4—Nb1ⁱ	72.78 (2)	C18B_f—C17B_f—H17C_f	110.0
Nb3—Cl5—Nb2	73.04 (2)	N11B_f—C17B_f—H17D_f	110.0
Nb1ⁱ—Cl6—Nb3	72.81 (2)	C18B_f—C17B_f—H17D_f	110.0
Nb4^v—Cl7—Nb4	72.93 (2)	H17C_f—C17B_f—H17D_f	108.4
Nb4—Cl8—Nb4^iv	72.84 (3)	N12B_f—C18B_f—C17B_f	112.4 (9)
C1—N1—Nb1	158.1 (3)	N12B_f—C18B_f—H18C_f	109.1
C2—N2—Nb2	143.3 (4)	C17B_f—C18B_f—H18C_f	109.1
C3—N3—Nb3	154.5 (3)	N12B_f—C18B_f—H18D_f	109.1
C4—N4—Nb4	146.7 (3)	C17B_f—C18B_f—H18D_f	109.1
C7—N5—C9	110.4 (7)	H18C_f—C18B_f—H18D_f	107.9
C7—N5—C5	109.4 (6)	C20B_f—C19B_f—N11B_f	109.0 (8)
C9—N5—C5	112.4 (9)	C20B_f—C19B_f—H19C_f	109.9
C7—N5—H5N	108.1	N11B_f—C19B_f—H19C_f	109.9
C9—N5—H5N	108.1	C20B_f—C19B_f—H19D_f	109.9
C5—N5—H5N	108.1	N11B_f—C19B_f—H19D_f	109.9
C6—N6—C10	107.9 (6)	H19C_f—C19B_f—H19D_f	108.3
C6—N6—C8	105.2 (5)	N12B_f—C20B_f—C19B_f	110 (1)
C10—N6—C8	105.1 (5)	N12B_f—C20B_f—H20C_f	109.6
C11—N7—C11^vi	108.6 (3)	C19B_f—C20B_f—H20C_f	109.6
C11—N7—C11^vii	108.6 (3)	N12B_f—C20B_f—H20D_f	109.6
C11^vi—N7—C11^vii	108.6 (3)	C19B_f—C20B_f—H20D_f	109.6
C12^vii—N8—C12^vi	108.6 (3)	H20C_f—C20B_f—H20D_f	108.1
C12^vii—N8—C12	108.6 (3)

Nb2—N2—C2—S2B_a	−156 (2)	C17A_e—N11A_e—C15A_e—C16A_e	−63 (1)
Nb3—N3—C3—S3A_c	−130 (2)	C20A_e—N12A_e—C16A_e—C15A_e	−60 (1)
Nb3—N3—C3—S3B_d	51 (3)	C18A_e—N12A_e—C16A_e—C15A_e	57 (1)
C7—N5—C5—C6	−75.1 (9)	N11A_e—C15A_e—C16A_e—N12A_e	3 (1)
C9—N5—C5—C6	48.0 (9)	C19A_e—N11A_e—C17A_e—C18A_e	−61 (1)
C10—N6—C6—C5	−68.9 (9)	C15A_e—N11A_e—C17A_e—C18A_e	60 (1)
C8—N6—C6—C5	42.8 (9)	N11A_e—C17A_e—C18A_e—N12A_e	3 (2)
N5—C5—C6—N6	22 (1)	C20A_e—N12A_e—C18A_e—C17A_e	56 (1)
C9—N5—C7—C8	−73.2 (9)	C16A_e—N12A_e—C18A_e—C17A_e	−61 (1)
C5—N5—C7—C8	51.2 (8)	C17A_e—N11A_e—C19A_e—C20A_e	58 (1)
N5—C7—C8—N6	19.7 (7)	C15A_e—N11A_e—C19A_e—C20A_e	−61 (1)
C6—N6—C8—C7	−67.5 (7)	C16A_e—N12A_e—C20A_e—C19A_e	58 (1)
C10—N6—C8—C7	46.2 (7)	C18A_e—N12A_e—C20A_e—C19A_e	−58 (1)
C7—N5—C9—C10	49 (1)	N11A_e—C19A_e—C20A_e—N12A_e	2 (1)
C5—N5—C9—C10	−73 (1)	C17B_f—N11B_f—C15B_f—C16B_f	67 (1)
C6—N6—C10—C9	40.7 (9)	C19B_f—N11B_f—C15B_f—C16B_f	−51 (1)
C8—N6—C10—C9	−71.2 (8)	C18B_f—N12B_f—C16B_f—C15B_f	−49 (2)
N5—C9—C10—N6	22 (1)	C20B_f—N12B_f—C16B_f—C15B_f	69 (1)
C11^vi—N7—C11—C12	−49.6 (5)	N11B_f—C15B_f—C16B_f—N12B_f	−14 (2)
C11^vii—N7—C11—C12	68.4 (5)	C15B_f—N11B_f—C17B_f—C18B_f	−52 (1)
C12^vii—N8—C12—C11	−49.6 (5)	C19B_f—N11B_f—C17B_f—C18B_f	64 (1)
C12^vi—N8—C12—C11	68.3 (4)	C20B_f—N12B_f—C18B_f—C17B_f	−51 (2)
N7—C11—C12—N8	−16.1 (5)	C16B_f—N12B_f—C18B_f—C17B_f	65 (2)
C13^vii—N9—C13—C14	69.6 (4)	N11B_f—C17B_f—C18B_f—N12B_f	−12 (2)
C13^vi—N9—C13—C14	−49.2 (4)	C17B_f—N11B_f—C19B_f—C20B_f	−49 (1)
C14^vii—N10—C14—C13	−49.7 (5)	C15B_f—N11B_f—C19B_f—C20B_f	68 (1)
C14^vi—N10—C14—C13	69.9 (4)	C18B_f—N12B_f—C20B_f—C19B_f	66 (1)
N9—C13—C14—N10	−17.3 (5)	C16B_f—N12B_f—C20B_f—C19B_f	−51 (1)
C19A_e—N11A_e—C15A_e—C16A_e	58 (1)	N11B_f—C19B_f—C20B_f—N12B_f	−15 (1)

Symmetry codes: (i) −x+1/3, −y+2/3, −z+2/3; (ii) −y+1, x−y, z; (iii) x−y+1/3, x−1/3, −z+2/3; (iv) y+1/3, −x+y+2/3, −z+2/3; (v) −x+y+1, −x+1, z; (vi) −x+y, −x+1, z; (vii) −y+1, x−y+1, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N5—H5N···Cl5	1.00	2.46	3.368 (7)	150
N8—H8N···N9	1.00	1.80	2.795 (8)	180
N10—H10N···Cl7^viii	1.00	2.90	3.695 (5)	137
N12A—H12N···N6ⁱⁱⁱ	1.00	1.59	2.59 (1)	176
N10—H10N···Cl7^ix	1.00	2.90	3.695 (5)	137
N10—H10N···Cl7^x	1.00	2.90	3.695 (5)	137

Symmetry codes: (iii) x−y+1/3, x−1/3, −z+2/3; (viii) −x+1, −y+1, −z+1; (ix) y, −x+y+1, −z+1; (x) x−y, x, −z+1.

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Tetra­kis(tri­ethyl­enediamin-1-ium) dodeca-μ2-chlorido-hexakis(thio­cyanato-κN)hexa-octa­hedro-niobate

Supporting information

Key indicators

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Tetrakis(triethylenediamin-1-ium) dodeca-μ₂-chlorido-hexakis(thiocyanato-κN)hexa-octahedro-niobate