Niobium isocyanide com­plexes, Nb(CNAr)6, with Ar = 2,6-di­methyl­phenyl (X­yl), a diamagnetic dimer containing four reductively coupled isocyanides, and Ar = 2,6-diiso­propyl­phenyl (Dipp), a paramagnetic monomer analogous to the highly unstable hexa­carbonyl­niobium(0)

Kucera, B.E.; Roberts, C.J.; Young Jr, V.G.; Brennessel, W.W.; Ellis, J.E.

doi:10.1107/S205322961901101X

Niobium isocyanide complexes, Nb(CNAr)₆, with Ar = 2,6-dimethylphenyl (Xyl), a diamagnetic dimer containing four reductively coupled isocyanides, and Ar = 2,6-diisopropylphenyl (Dipp), a paramagnetic monomer analogous to the highly unstable hexacarbonylniobium(0)

B. E. Kucera, C. J. Roberts, V. G. Young Jr, W. W. Brennessel and J. E. Ellis

Treatment of bis(mesitylene)niobium(0) with 6–7 equivalents of 2,6-dimethylphenyl isocyanide (CNXyl) affords two products with the empirical formula Nb(CNXyl)_n (n = 7 or 6), which have been shown to be the diamagnetic dimers bis[μ-N,N′,N′′,N′′′-tetrakis(2,6-dimethylphenyl)squaramidinato(2−)]bis[pentakis(2,6-dimethylphenyl isocyanide)niobium(I)], [Nb₂(C₉H₉N)₁₀(C₃₆H₃₆N₄)] or [Nb(CNXyl)₅]₂[μ-C₄(NXyl)₄]·xSolvent, 1, and bis[μ-N,N′,N′′,N′′′-tetrakis(2,6-dimethylphenyl)squaramidinato(2−)]bis[tetrakis(2,6-dimethylphenyl isocyanide)niobium(I)] tetrahydrofuran trisolvate, [Nb₂(C₉H₉N)₈(C₃₆H₃₆N₄)]·3C₄H₈O or [Nb(CNXyl)₄]₂[μ-C₄(NXyl)₄]·3THF (THF = tetrahydrofuran), 2. Each contains Nb^I bound to either five or four terminal isocyanides, respectively, and to an unprecedented bridging tetraarylsquaramidinate(2−) unit, coordinated as a bidentate ligand to each niobium center, symmetrically due to the crystallographic inversion center that coincides with the centroid of the central C₄ unit. Thus, in the presence of CNXyl, the bis(mesitylene)niobium(0) is oxidized to niobium(I), resulting in the facile loss of both mesitylene groups and the reductive coupling of two CNXyl groups per niobium to provide the first examples of tetraarylsquaramidinate(2−) ligands, [cyclo-C₄N₄Ar₄]²⁻, coordinated to metals. In contrast, bis(mesitylene)niobium(0) reacts with the more crowded 2,6-diisopropylphenyl isocyanide (CNDipp) to afford the paramagnetic monomer hexakis(2,6-diisopropylphenyl isocyanide)niobium(0), [Nb(C₁₃H₁₇N)₆] or Nb(CNDipp)₆, 3, the first zero-valent niobium isocyanide analog of the highly unstable Nb(CO)₆, which is presently only known to exist in an argon matrix at 4.2 K.

Keywords: isocyanide; 2,6-dimethylphenyl isocyanide; 2,6-diisopropylphenyl isocyanide; squarate; squaramidinate; low-valent; niobium; crystal structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S205322961901101X/qf3033sup1.cif Contains datablocks 1, 2, 3, global
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961901101X/qf30331sup2.hkl Contains datablock 1
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961901101X/qf30332sup3.hkl Contains datablock 2
	Structure factor file (CIF format) https://doi.org/10.1107/S205322961901101X/qf30333sup4.hkl Contains datablock 3
	Portable Document Format (PDF) file https://doi.org/10.1107/S205322961901101X/qf3033sup5.pdf IR spectral data

CCDC references: 1945886; 1945885; 1945884

Computing details top

Data collection: SMART (Bruker, 2003) for (1), (2); APEX2 (Bruker, 2013) for (3). Cell refinement: SAINT (Bruker, 2003) for (1), (2); SAINT (Bruker, 2013) for (3). Data reduction: SAINT (Bruker, 2003) for (1), (2); SAINT (Bruker, 2013) for (3). For all structures, program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Bis[µ-N,N',N'',N'''-tetrakis(2,6-\ dimethylphenyl)squaramidinato(2-)]bis[pentakis(2,6-dimethylphenyl isocyanide)niobium(I)] (1) top

Crystal data top

[Nb₂(C₉H₉N)₁₀(C₃₆H₃₆N₄)]	F(000) = 4248
M_r = 2022.22	D_x = 1.076 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 32.077 (5) Å	Cell parameters from 3690 reflections
b = 15.830 (2) Å	θ = 2.3–23.5°
c = 24.815 (4) Å	µ = 0.23 mm⁻¹
β = 97.655 (2)°	T = 173 K
V = 12488 (3) Å³	Plate, green-black
Z = 4	0.50 × 0.50 × 0.20 mm

Data collection top

Bruker SMART CCD platform diffractometer	6478 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tube	R_int = 0.051
ω scans	θ_max = 25.1°, θ_min = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −24→38
T_min = 0.893, T_max = 0.955	k = −17→18
22038 measured reflections	l = −17→29
10394 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)] = 0.055	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.144	H-atom parameters constrained
S = 1.00	w = 1/[σ²(F_o²) + (0.0754P)²] where P = (F_o² + 2F_c²)/3
10394 reflections	(Δ/σ)_max = 0.001
773 parameters	Δρ_max = 0.38 e Å⁻³
462 restraints	Δρ_min = −0.25 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. Reflection contributions from highly disordered solvent were fixed and added to the calculated structure factors using the SQUEEZE routine of program Platon (Spek, 2015), which determined there to be 408 electrons in 1634 Å³ treated this way per unit cell. Because the exact identity and amount of solvent were unknown, no solvent was included in the atom list or molecular formula. Thus all calculated quantities that derive from the molecular formula (e.g., F(000), density, molecular weight, etc.) are known to be incorrect.

2,6-dimethylphenyl group C8-C15 is modeled as disordered over two positions (0.570 (7):0.430 (7)). Isocyanide ligand C7/N7/C57-C63 is modeled as disordered over four positions as an approximation for what appears to be a frozen dynamic disorder (0.417 (3):0.331 (3):0.185 (3):0.067 (3)). For each site of disorder, analogous bond lengths and angles were restrained to be similar. Anisotropic displacement parameters for proximal and related atoms were restrained to be similar and/or constrained to be equivalent.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Nb1	0.11101 (2)	0.48958 (2)	0.98057 (2)	0.03672 (13)
N1	0.04468 (9)	0.4410 (2)	0.94357 (13)	0.0428 (8)
N2	0.06582 (9)	0.55025 (19)	1.03720 (12)	0.0369 (7)
N3	0.19727 (12)	0.5470 (2)	0.93368 (16)	0.0600 (10)
N4	0.18134 (10)	0.5429 (2)	1.08353 (14)	0.0499 (9)
N5	0.14160 (10)	0.3377 (2)	0.90392 (15)	0.0499 (9)
N6	0.13805 (10)	0.3208 (2)	1.05731 (15)	0.0480 (9)
C1	0.01683 (11)	0.4716 (2)	0.97262 (15)	0.0360 (9)
C2	0.02745 (11)	0.5256 (2)	1.01901 (15)	0.0353 (9)
C3	0.16549 (13)	0.5279 (2)	0.95014 (17)	0.0436 (10)
C4	0.15651 (11)	0.5265 (2)	1.04569 (16)	0.0392 (9)
C5	0.13066 (11)	0.3942 (3)	0.92927 (17)	0.0412 (10)
C6	0.12637 (11)	0.3801 (3)	1.03103 (16)	0.0394 (9)
C8	0.0355 (10)	0.3598 (7)	0.9174 (5)	0.041 (2)	0.430 (7)
C9	0.0264 (9)	0.2836 (10)	0.9428 (6)	0.049 (3)	0.430 (7)
C10	0.0192 (8)	0.2101 (10)	0.9109 (6)	0.079 (4)	0.430 (7)
H10	0.012406	0.158791	0.927615	0.094*	0.430 (7)
C11	0.0218 (6)	0.2110 (9)	0.8548 (6)	0.084 (4)	0.430 (7)
H11	0.017064	0.160482	0.834290	0.100*	0.430 (7)
C12	0.0313 (8)	0.2860 (10)	0.8290 (6)	0.083 (4)	0.430 (7)
H12	0.033698	0.287014	0.791227	0.100*	0.430 (7)
C13	0.0372 (6)	0.3595 (8)	0.8606 (5)	0.046 (3)	0.430 (7)
C14	0.0222 (12)	0.282 (2)	1.0021 (7)	0.063 (4)	0.430 (7)
H14A	0.047974	0.304354	1.022962	0.094*	0.430 (7)
H14B	0.017459	0.224223	1.013488	0.094*	0.430 (7)
H14C	−0.001732	0.317658	1.008756	0.094*	0.430 (7)
C15	0.0452 (7)	0.4396 (11)	0.8316 (8)	0.063 (3)	0.430 (7)
H15A	0.022617	0.480050	0.835061	0.094*	0.430 (7)
H15B	0.046218	0.427519	0.793060	0.094*	0.430 (7)
H15C	0.072192	0.463735	0.847712	0.094*	0.430 (7)
C8'	0.0339 (7)	0.3790 (5)	0.9015 (3)	0.041 (2)	0.570 (7)
C9'	0.0261 (6)	0.2992 (7)	0.9210 (4)	0.049 (3)	0.570 (7)
C10'	0.0197 (5)	0.2332 (8)	0.8825 (5)	0.079 (4)	0.570 (7)
H10'	0.014203	0.177333	0.893628	0.094*	0.570 (7)
C11'	0.0215 (4)	0.2511 (7)	0.8279 (5)	0.084 (4)	0.570 (7)
H11'	0.016482	0.206766	0.802081	0.100*	0.570 (7)
C12'	0.0302 (5)	0.3314 (7)	0.8099 (5)	0.083 (4)	0.570 (7)
H12'	0.031684	0.340935	0.772420	0.100*	0.570 (7)
C13'	0.0369 (4)	0.3979 (6)	0.8469 (4)	0.046 (3)	0.570 (7)
C14'	0.0263 (9)	0.2789 (16)	0.9802 (5)	0.063 (4)	0.570 (7)
H14D	0.052469	0.299260	1.000912	0.094*	0.570 (7)
H14E	0.024130	0.217617	0.984690	0.094*	0.570 (7)
H14F	0.002269	0.306539	0.993459	0.094*	0.570 (7)
C15'	0.0452 (5)	0.4856 (7)	0.8286 (6)	0.063 (3)	0.570 (7)
H15D	0.030193	0.526137	0.848859	0.094*	0.570 (7)
H15E	0.035325	0.490989	0.789634	0.094*	0.570 (7)
H15F	0.075446	0.497160	0.835292	0.094*	0.570 (7)
C16	0.07426 (11)	0.5846 (3)	1.09123 (16)	0.0420 (10)
C17	0.07078 (13)	0.5331 (3)	1.13580 (18)	0.0549 (12)
C18	0.08118 (16)	0.5678 (4)	1.1880 (2)	0.0786 (16)
H18	0.078891	0.534016	1.219111	0.094*
C19	0.09474 (16)	0.6509 (4)	1.1946 (2)	0.0847 (18)
H19	0.101076	0.674062	1.230109	0.102*
C20	0.09887 (14)	0.6983 (4)	1.1511 (2)	0.0727 (15)
H20	0.108911	0.754551	1.156327	0.087*
C21	0.08891 (13)	0.6678 (3)	1.0982 (2)	0.0564 (12)
C22	0.05723 (16)	0.4428 (3)	1.1288 (2)	0.0740 (15)
H22A	0.028016	0.440492	1.111220	0.111*
H22B	0.059411	0.415370	1.164422	0.111*
H22C	0.075398	0.413516	1.106035	0.111*
C23	0.09445 (16)	0.7228 (3)	1.0511 (2)	0.0769 (16)
H23A	0.106432	0.777092	1.064364	0.115*
H23B	0.067100	0.732299	1.029247	0.115*
H23C	0.113478	0.695305	1.028760	0.115*
C24	0.23068 (13)	0.5715 (3)	0.9067 (2)	0.0522 (11)
C25	0.22221 (15)	0.6082 (3)	0.8558 (2)	0.0617 (13)
C26	0.25588 (19)	0.6324 (3)	0.8300 (2)	0.0801 (16)
H26	0.250920	0.657956	0.795068	0.096*
C27	0.2964 (2)	0.6198 (4)	0.8541 (3)	0.0875 (19)
H27	0.319088	0.636749	0.835677	0.105*
C28	0.30469 (15)	0.5831 (3)	0.9045 (3)	0.0777 (17)
H28	0.332990	0.575502	0.920724	0.093*
C29	0.27134 (15)	0.5566 (3)	0.9325 (2)	0.0632 (13)
C30	0.17781 (16)	0.6246 (3)	0.8284 (2)	0.0800 (16)
H30A	0.163339	0.662148	0.851231	0.120*
H30B	0.162537	0.570936	0.823299	0.120*
H30C	0.178880	0.651206	0.792966	0.120*
C31	0.27966 (17)	0.5121 (3)	0.9868 (3)	0.0856 (17)
H31A	0.264747	0.541501	1.013302	0.128*
H31B	0.309925	0.512470	0.999493	0.128*
H31C	0.269685	0.453670	0.982848	0.128*
C32	0.21258 (11)	0.5657 (3)	1.12518 (17)	0.0435 (10)
C33	0.23594 (14)	0.6372 (3)	1.11786 (18)	0.0562 (12)
C34	0.26788 (16)	0.6569 (3)	1.1595 (2)	0.0782 (16)
H34	0.284997	0.705037	1.155943	0.094*
C35	0.27522 (16)	0.6085 (3)	1.2055 (2)	0.0752 (15)
H35	0.297612	0.622822	1.233018	0.090*
C36	0.25077 (14)	0.5400 (3)	1.21227 (18)	0.0598 (12)
H36	0.255600	0.508396	1.245067	0.072*
C37	0.21904 (13)	0.5158 (3)	1.17208 (17)	0.0517 (11)
C38	0.22611 (16)	0.6916 (3)	1.0681 (2)	0.0761 (15)
H38A	0.196733	0.710177	1.064873	0.114*
H38B	0.230562	0.659100	1.035783	0.114*
H38C	0.244634	0.741124	1.071316	0.114*
C39	0.19141 (16)	0.4412 (3)	1.1790 (2)	0.0798 (16)
H39A	0.192979	0.427466	1.217751	0.120*
H39B	0.200909	0.392608	1.159440	0.120*
H39C	0.162282	0.454815	1.164423	0.120*
C40	0.15562 (12)	0.2774 (3)	0.86965 (18)	0.0478 (11)
C41	0.15487 (14)	0.1917 (3)	0.8852 (2)	0.0605 (13)
C42	0.17149 (17)	0.1336 (3)	0.8512 (3)	0.0813 (16)
H42	0.172977	0.075478	0.860733	0.098*
C43	0.18571 (19)	0.1603 (4)	0.8040 (3)	0.0940 (19)
H43	0.195791	0.119527	0.780774	0.113*
C44	0.18570 (16)	0.2437 (4)	0.7897 (2)	0.0753 (15)
H44	0.196412	0.260102	0.757344	0.090*
C45	0.17022 (13)	0.3044 (3)	0.82190 (19)	0.0573 (12)
C46	0.13898 (16)	0.1665 (3)	0.9369 (2)	0.0768 (15)
H46A	0.137305	0.104734	0.938756	0.115*
H46B	0.110978	0.190715	0.937850	0.115*
H46C	0.158262	0.187394	0.968012	0.115*
C47	0.17069 (15)	0.3965 (3)	0.8075 (2)	0.0734 (14)
H47A	0.142717	0.420719	0.808821	0.110*
H47B	0.178310	0.402952	0.770777	0.110*
H47C	0.191338	0.426044	0.833546	0.110*
C48	0.16300 (13)	0.2566 (3)	1.08325 (17)	0.0483 (11)
C49	0.20542 (13)	0.2554 (3)	1.07676 (18)	0.0510 (11)
C50	0.22961 (14)	0.1910 (3)	1.1029 (2)	0.0629 (13)
H50	0.258806	0.188371	1.099967	0.075*
C51	0.21204 (16)	0.1307 (3)	1.1332 (2)	0.0678 (14)
H51	0.229002	0.086266	1.149847	0.081*
C52	0.17053 (16)	0.1346 (3)	1.1393 (2)	0.0693 (14)
H52	0.159028	0.093438	1.160954	0.083*
C53	0.14477 (14)	0.1976 (3)	1.1144 (2)	0.0647 (13)
C54	0.22421 (13)	0.3223 (3)	1.0446 (2)	0.0665 (14)
H54A	0.210272	0.321568	1.007004	0.100*
H54B	0.254325	0.311321	1.045103	0.100*
H54C	0.220316	0.377787	1.060765	0.100*
C55	0.09883 (17)	0.2029 (4)	1.1206 (3)	0.121 (3)
H55A	0.092441	0.259468	1.133293	0.182*
H55B	0.092204	0.160743	1.147139	0.182*
H55C	0.081906	0.191894	1.085449	0.182*
C7	0.099 (8)	0.609 (3)	0.933 (3)	0.046 (3)	0.067 (3)
N7	0.097 (2)	0.6814 (17)	0.9198 (19)	0.049 (3)	0.067 (3)
C56	0.0849 (14)	0.7695 (17)	0.9243 (13)	0.082 (3)	0.067 (3)
C57	0.1154 (13)	0.826 (3)	0.9496 (16)	0.084 (4)	0.067 (3)
C58	0.1033 (19)	0.912 (3)	0.954 (2)	0.130 (6)	0.067 (3)
H58	0.123482	0.950674	0.970656	0.156*	0.067 (3)
C59	0.063 (2)	0.941 (3)	0.934 (3)	0.149 (6)	0.067 (3)
H59	0.055810	0.998920	0.937324	0.179*	0.067 (3)
C60	0.0345 (16)	0.882 (3)	0.909 (3)	0.142 (6)	0.067 (3)
H60	0.007037	0.901199	0.895707	0.170*	0.067 (3)
C61	0.0441 (14)	0.795 (3)	0.904 (2)	0.114 (5)	0.067 (3)
C62	0.1607 (14)	0.812 (5)	0.975 (2)	0.068 (4)	0.067 (3)
H62A	0.172595	0.866370	0.988740	0.102*	0.067 (3)
H62B	0.161653	0.771646	1.004501	0.102*	0.067 (3)
H62C	0.177001	0.790896	0.946965	0.102*	0.067 (3)
C63	0.011 (4)	0.735 (8)	0.876 (3)	0.136 (7)	0.067 (3)
H63A	−0.014840	0.765533	0.864907	0.204*	0.067 (3)
H63B	0.021528	0.709341	0.844650	0.204*	0.067 (3)
H63C	0.006177	0.690375	0.902222	0.204*	0.067 (3)
C7'	0.092 (2)	0.607 (3)	0.933 (3)	0.046 (3)	0.331 (3)
N7'	0.0917 (10)	0.6715 (9)	0.9090 (9)	0.049 (3)	0.331 (3)
C56'	0.0871 (7)	0.7626 (10)	0.9009 (6)	0.082 (3)	0.331 (3)
C57'	0.1218 (7)	0.8145 (13)	0.9185 (7)	0.084 (4)	0.331 (3)
C58'	0.1159 (7)	0.9025 (13)	0.9097 (8)	0.130 (6)	0.331 (3)
H58'	0.138934	0.938998	0.920918	0.156*	0.331 (3)
C59'	0.0785 (6)	0.9387 (12)	0.8855 (8)	0.149 (6)	0.331 (3)
H59'	0.075713	0.998074	0.880839	0.179*	0.331 (3)
C60'	0.0451 (6)	0.8839 (12)	0.8685 (8)	0.142 (6)	0.331 (3)
H60'	0.019317	0.906784	0.851430	0.170*	0.331 (3)
C61'	0.0487 (7)	0.7951 (11)	0.8761 (7)	0.114 (5)	0.331 (3)
C62'	0.1600 (9)	0.765 (2)	0.9445 (11)	0.068 (4)	0.331 (3)
H62D	0.183107	0.804264	0.956016	0.102*	0.331 (3)
H62E	0.152729	0.734218	0.976238	0.102*	0.331 (3)
H62F	0.168647	0.724951	0.918085	0.102*	0.331 (3)
C63'	0.0133 (12)	0.735 (3)	0.8587 (11)	0.136 (7)	0.331 (3)
H63D	−0.011387	0.766297	0.842090	0.204*	0.331 (3)
H63E	0.021991	0.694750	0.832107	0.204*	0.331 (3)
H63F	0.006288	0.703668	0.890411	0.204*	0.331 (3)
C7"	0.096 (2)	0.6074 (19)	0.932 (2)	0.046 (3)	0.417 (3)
N7"	0.0852 (8)	0.6754 (7)	0.9164 (7)	0.049 (3)	0.417 (3)
C56"	0.0869 (5)	0.7569 (8)	0.8900 (5)	0.082 (3)	0.417 (3)
C57"	0.1227 (5)	0.8071 (9)	0.9051 (6)	0.084 (4)	0.417 (3)
C58"	0.1236 (5)	0.8856 (10)	0.8787 (6)	0.130 (6)	0.417 (3)
H58"	0.147419	0.921210	0.887541	0.156*	0.417 (3)
C59"	0.0907 (5)	0.9130 (10)	0.8399 (6)	0.149 (6)	0.417 (3)
H59"	0.091979	0.966713	0.823100	0.179*	0.417 (3)
C60"	0.0560 (5)	0.8608 (10)	0.8263 (6)	0.142 (6)	0.417 (3)
H60"	0.033831	0.879280	0.799691	0.170*	0.417 (3)
C61"	0.0529 (5)	0.7805 (9)	0.8511 (6)	0.114 (5)	0.417 (3)
C62"	0.1614 (7)	0.7890 (16)	0.9466 (9)	0.068 (4)	0.417 (3)
H62G	0.180962	0.836760	0.947746	0.102*	0.417 (3)
H62H	0.152729	0.780870	0.982629	0.102*	0.417 (3)
H62I	0.175419	0.737718	0.935976	0.102*	0.417 (3)
C63"	0.0150 (8)	0.724 (2)	0.8363 (10)	0.136 (7)	0.417 (3)
H63G	−0.004897	0.752473	0.808647	0.204*	0.417 (3)
H63H	0.023975	0.670710	0.822012	0.204*	0.417 (3)
H63I	0.001420	0.713867	0.868785	0.204*	0.417 (3)
C7Z	0.088 (2)	0.603 (4)	0.932 (3)	0.046 (3)	0.185 (3)
N7Z	0.0840 (8)	0.6559 (11)	0.8977 (9)	0.049 (3)	0.185 (3)
C56Z	0.0915 (5)	0.7233 (10)	0.8621 (7)	0.082 (3)	0.185 (3)
C57Z	0.1208 (7)	0.7867 (13)	0.8794 (9)	0.084 (4)	0.185 (3)
C58Z	0.1249 (8)	0.8498 (15)	0.8395 (11)	0.130 (6)	0.185 (3)
H58Z	0.144201	0.894692	0.848705	0.156*	0.185 (3)
C59Z	0.1019 (8)	0.8493 (16)	0.7873 (11)	0.149 (6)	0.185 (3)
H59Z	0.105583	0.892851	0.762022	0.179*	0.185 (3)
C60Z	0.0736 (7)	0.7834 (16)	0.7731 (10)	0.142 (6)	0.185 (3)
H60Z	0.058082	0.782070	0.737704	0.170*	0.185 (3)
C61Z	0.0677 (6)	0.7188 (13)	0.8106 (8)	0.114 (5)	0.185 (3)
C62Z	0.1454 (11)	0.786 (3)	0.9363 (12)	0.068 (4)	0.185 (3)
H62J	0.164119	0.835414	0.940657	0.102*	0.185 (3)
H62K	0.125727	0.788780	0.963285	0.102*	0.185 (3)
H62L	0.162091	0.734416	0.941510	0.102*	0.185 (3)
C63Z	0.0363 (7)	0.6489 (17)	0.7950 (14)	0.136 (7)	0.185 (3)
H63J	0.023055	0.657286	0.757486	0.204*	0.185 (3)
H63K	0.050857	0.594270	0.797973	0.204*	0.185 (3)
H63L	0.014728	0.649661	0.819467	0.204*	0.185 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Nb1	0.02807 (18)	0.0448 (2)	0.0384 (2)	0.00011 (16)	0.00866 (14)	−0.00220 (18)
N1	0.0296 (18)	0.060 (2)	0.0391 (19)	−0.0040 (15)	0.0063 (15)	−0.0181 (17)
N2	0.0259 (16)	0.0480 (19)	0.0372 (19)	−0.0011 (14)	0.0062 (14)	−0.0073 (15)
N3	0.054 (2)	0.061 (2)	0.072 (3)	−0.0142 (19)	0.031 (2)	−0.010 (2)
N4	0.0311 (18)	0.068 (2)	0.050 (2)	0.0029 (16)	0.0065 (17)	−0.0074 (19)
N5	0.0361 (19)	0.055 (2)	0.060 (2)	0.0042 (17)	0.0107 (17)	−0.0124 (19)
N6	0.0341 (19)	0.047 (2)	0.063 (2)	−0.0007 (16)	0.0087 (17)	0.0086 (19)
C1	0.029 (2)	0.041 (2)	0.038 (2)	0.0023 (17)	0.0061 (18)	−0.0022 (17)
C2	0.029 (2)	0.041 (2)	0.037 (2)	−0.0015 (16)	0.0059 (16)	−0.0051 (17)
C3	0.039 (2)	0.043 (2)	0.050 (3)	−0.0028 (19)	0.009 (2)	−0.0064 (19)
C4	0.030 (2)	0.046 (2)	0.044 (2)	0.0052 (17)	0.0131 (19)	0.0015 (19)
C5	0.028 (2)	0.048 (3)	0.048 (3)	−0.0010 (18)	0.0073 (18)	0.002 (2)
C6	0.027 (2)	0.045 (2)	0.047 (3)	−0.0026 (17)	0.0099 (18)	−0.003 (2)
C8	0.027 (3)	0.066 (5)	0.029 (6)	0.012 (5)	0.000 (7)	0.000 (5)
C9	0.041 (3)	0.057 (6)	0.048 (8)	0.005 (4)	0.000 (8)	−0.009 (6)
C10	0.066 (4)	0.069 (8)	0.095 (11)	0.002 (6)	−0.011 (10)	−0.033 (7)
C11	0.081 (5)	0.077 (9)	0.087 (10)	0.004 (7)	−0.010 (8)	−0.041 (7)
C12	0.078 (5)	0.114 (11)	0.061 (8)	−0.018 (10)	0.021 (7)	−0.037 (7)
C13	0.036 (3)	0.062 (8)	0.038 (6)	−0.001 (7)	0.007 (4)	−0.004 (5)
C14	0.056 (6)	0.054 (4)	0.082 (12)	−0.008 (4)	0.022 (11)	−0.001 (11)
C15	0.062 (4)	0.090 (10)	0.037 (3)	−0.003 (9)	0.009 (3)	0.000 (8)
C8'	0.027 (3)	0.066 (5)	0.029 (6)	0.012 (5)	0.000 (7)	0.000 (5)
C9'	0.041 (3)	0.057 (6)	0.048 (8)	0.005 (4)	0.000 (8)	−0.009 (6)
C10'	0.066 (4)	0.069 (8)	0.095 (11)	0.002 (6)	−0.011 (10)	−0.033 (7)
C11'	0.081 (5)	0.077 (9)	0.087 (10)	0.004 (7)	−0.010 (8)	−0.041 (7)
C12'	0.078 (5)	0.114 (11)	0.061 (8)	−0.018 (10)	0.021 (7)	−0.037 (7)
C13'	0.036 (3)	0.062 (8)	0.038 (6)	−0.001 (7)	0.007 (4)	−0.004 (5)
C14'	0.056 (6)	0.054 (4)	0.082 (12)	−0.008 (4)	0.022 (11)	−0.001 (11)
C15'	0.062 (4)	0.090 (10)	0.037 (3)	−0.003 (9)	0.009 (3)	0.000 (8)
C16	0.025 (2)	0.061 (3)	0.041 (2)	0.0010 (18)	0.0073 (18)	−0.015 (2)
C17	0.047 (3)	0.078 (4)	0.040 (3)	0.009 (2)	0.010 (2)	−0.005 (2)
C18	0.073 (4)	0.122 (5)	0.041 (3)	0.017 (3)	0.010 (3)	−0.005 (3)
C19	0.070 (4)	0.122 (5)	0.058 (4)	0.006 (3)	−0.006 (3)	−0.048 (4)
C20	0.055 (3)	0.091 (4)	0.070 (4)	−0.002 (3)	0.002 (3)	−0.041 (3)
C21	0.040 (2)	0.068 (3)	0.060 (3)	0.003 (2)	0.006 (2)	−0.022 (3)
C22	0.086 (4)	0.085 (4)	0.056 (3)	0.010 (3)	0.030 (3)	0.015 (3)
C23	0.078 (4)	0.055 (3)	0.099 (4)	−0.014 (3)	0.018 (3)	−0.020 (3)
C24	0.044 (3)	0.048 (3)	0.070 (3)	−0.016 (2)	0.025 (2)	−0.015 (2)
C25	0.069 (3)	0.062 (3)	0.060 (3)	−0.018 (2)	0.029 (3)	−0.010 (3)
C26	0.087 (4)	0.086 (4)	0.075 (4)	−0.019 (3)	0.041 (4)	−0.009 (3)
C27	0.090 (5)	0.071 (4)	0.116 (6)	−0.022 (3)	0.067 (4)	−0.009 (4)
C28	0.049 (3)	0.060 (3)	0.130 (6)	−0.011 (2)	0.036 (3)	−0.015 (3)
C29	0.058 (3)	0.052 (3)	0.085 (4)	−0.011 (2)	0.030 (3)	−0.016 (3)
C30	0.091 (4)	0.085 (4)	0.063 (4)	−0.022 (3)	0.008 (3)	−0.006 (3)
C31	0.075 (4)	0.068 (4)	0.115 (5)	0.008 (3)	0.017 (3)	0.001 (3)
C32	0.035 (2)	0.046 (3)	0.049 (3)	0.0054 (18)	0.0016 (19)	−0.014 (2)
C33	0.060 (3)	0.047 (3)	0.058 (3)	0.002 (2)	−0.008 (2)	−0.005 (2)
C34	0.093 (4)	0.063 (3)	0.072 (4)	−0.027 (3)	−0.016 (3)	−0.002 (3)
C35	0.077 (4)	0.078 (4)	0.062 (4)	−0.014 (3)	−0.024 (3)	−0.005 (3)
C36	0.070 (3)	0.065 (3)	0.042 (3)	0.005 (2)	0.001 (2)	−0.003 (2)
C37	0.053 (3)	0.061 (3)	0.043 (2)	0.004 (2)	0.011 (2)	−0.005 (2)
C38	0.093 (4)	0.058 (3)	0.071 (4)	−0.011 (3)	−0.010 (3)	0.003 (3)
C39	0.089 (4)	0.099 (4)	0.054 (3)	−0.024 (3)	0.018 (3)	0.001 (3)
C40	0.033 (2)	0.053 (3)	0.058 (3)	0.0035 (19)	0.004 (2)	−0.015 (2)
C41	0.049 (3)	0.063 (3)	0.069 (3)	0.002 (2)	0.006 (2)	−0.005 (3)
C42	0.092 (4)	0.056 (3)	0.096 (5)	0.012 (3)	0.011 (4)	−0.017 (3)
C43	0.114 (5)	0.091 (5)	0.082 (5)	0.033 (4)	0.029 (4)	−0.026 (4)
C44	0.085 (4)	0.081 (4)	0.064 (4)	0.020 (3)	0.025 (3)	−0.011 (3)
C45	0.045 (3)	0.069 (3)	0.059 (3)	0.006 (2)	0.009 (2)	−0.012 (3)
C46	0.076 (4)	0.064 (3)	0.091 (4)	−0.004 (3)	0.014 (3)	0.005 (3)
C47	0.076 (3)	0.067 (3)	0.080 (4)	−0.007 (3)	0.017 (3)	−0.008 (3)
C48	0.042 (2)	0.047 (3)	0.056 (3)	0.004 (2)	0.005 (2)	0.004 (2)
C49	0.042 (2)	0.057 (3)	0.054 (3)	0.005 (2)	0.005 (2)	0.001 (2)
C50	0.045 (3)	0.075 (3)	0.068 (3)	0.012 (2)	0.003 (2)	0.002 (3)
C51	0.067 (4)	0.068 (3)	0.066 (3)	0.016 (3)	−0.002 (3)	0.011 (3)
C52	0.075 (4)	0.054 (3)	0.079 (4)	0.002 (3)	0.008 (3)	0.023 (3)
C53	0.055 (3)	0.057 (3)	0.081 (4)	0.005 (2)	0.004 (3)	0.019 (3)
C54	0.041 (3)	0.087 (4)	0.073 (4)	0.008 (2)	0.014 (2)	0.015 (3)
C55	0.066 (4)	0.119 (5)	0.183 (7)	0.000 (3)	0.035 (4)	0.087 (5)
C7	0.031 (7)	0.057 (3)	0.050 (3)	−0.001 (3)	0.007 (5)	0.008 (2)
N7	0.034 (6)	0.061 (3)	0.054 (4)	−0.003 (3)	0.005 (4)	0.015 (3)
C56	0.078 (4)	0.084 (5)	0.082 (8)	0.000 (4)	0.000 (5)	0.043 (5)
C57	0.087 (5)	0.072 (6)	0.090 (10)	−0.013 (4)	0.000 (7)	0.037 (7)
C58	0.153 (9)	0.101 (9)	0.127 (15)	−0.052 (7)	−0.012 (11)	0.071 (10)
C59	0.144 (10)	0.104 (9)	0.186 (14)	−0.021 (8)	−0.025 (11)	0.102 (10)
C60	0.117 (9)	0.121 (9)	0.177 (14)	0.004 (7)	−0.023 (10)	0.109 (10)
C61	0.092 (7)	0.102 (7)	0.138 (13)	−0.012 (5)	−0.017 (9)	0.073 (8)
C62	0.061 (6)	0.046 (11)	0.092 (6)	−0.016 (8)	−0.006 (4)	−0.007 (6)
C63	0.083 (6)	0.155 (10)	0.16 (2)	−0.009 (6)	−0.037 (11)	0.092 (12)
C7'	0.031 (7)	0.057 (3)	0.050 (3)	−0.001 (3)	0.007 (5)	0.008 (2)
N7'	0.034 (6)	0.061 (3)	0.054 (4)	−0.003 (3)	0.005 (4)	0.015 (3)
C56'	0.078 (4)	0.084 (5)	0.082 (8)	0.000 (4)	0.000 (5)	0.043 (5)
C57'	0.087 (5)	0.072 (6)	0.090 (10)	−0.013 (4)	0.000 (7)	0.037 (7)
C58'	0.153 (9)	0.101 (9)	0.127 (15)	−0.052 (7)	−0.012 (11)	0.071 (10)
C59'	0.144 (10)	0.104 (9)	0.186 (14)	−0.021 (8)	−0.025 (11)	0.102 (10)
C60'	0.117 (9)	0.121 (9)	0.177 (14)	0.004 (7)	−0.023 (10)	0.109 (10)
C61'	0.092 (7)	0.102 (7)	0.138 (13)	−0.012 (5)	−0.017 (9)	0.073 (8)
C62'	0.061 (6)	0.046 (11)	0.092 (6)	−0.016 (8)	−0.006 (4)	−0.007 (6)
C63'	0.083 (6)	0.155 (10)	0.16 (2)	−0.009 (6)	−0.037 (11)	0.092 (12)
C7"	0.031 (7)	0.057 (3)	0.050 (3)	−0.001 (3)	0.007 (5)	0.008 (2)
N7"	0.034 (6)	0.061 (3)	0.054 (4)	−0.003 (3)	0.005 (4)	0.015 (3)
C56"	0.078 (4)	0.084 (5)	0.082 (8)	0.000 (4)	0.000 (5)	0.043 (5)
C57"	0.087 (5)	0.072 (6)	0.090 (10)	−0.013 (4)	0.000 (7)	0.037 (7)
C58"	0.153 (9)	0.101 (9)	0.127 (15)	−0.052 (7)	−0.012 (11)	0.071 (10)
C59"	0.144 (10)	0.104 (9)	0.186 (14)	−0.021 (8)	−0.025 (11)	0.102 (10)
C60"	0.117 (9)	0.121 (9)	0.177 (14)	0.004 (7)	−0.023 (10)	0.109 (10)
C61"	0.092 (7)	0.102 (7)	0.138 (13)	−0.012 (5)	−0.017 (9)	0.073 (8)
C62"	0.061 (6)	0.046 (11)	0.092 (6)	−0.016 (8)	−0.006 (4)	−0.007 (6)
C63"	0.083 (6)	0.155 (10)	0.16 (2)	−0.009 (6)	−0.037 (11)	0.092 (12)
C7Z	0.031 (7)	0.057 (3)	0.050 (3)	−0.001 (3)	0.007 (5)	0.008 (2)
N7Z	0.034 (6)	0.061 (3)	0.054 (4)	−0.003 (3)	0.005 (4)	0.015 (3)
C56Z	0.078 (4)	0.084 (5)	0.082 (8)	0.000 (4)	0.000 (5)	0.043 (5)
C57Z	0.087 (5)	0.072 (6)	0.090 (10)	−0.013 (4)	0.000 (7)	0.037 (7)
C58Z	0.153 (9)	0.101 (9)	0.127 (15)	−0.052 (7)	−0.012 (11)	0.071 (10)
C59Z	0.144 (10)	0.104 (9)	0.186 (14)	−0.021 (8)	−0.025 (11)	0.102 (10)
C60Z	0.117 (9)	0.121 (9)	0.177 (14)	0.004 (7)	−0.023 (10)	0.109 (10)
C61Z	0.092 (7)	0.102 (7)	0.138 (13)	−0.012 (5)	−0.017 (9)	0.073 (8)
C62Z	0.061 (6)	0.046 (11)	0.092 (6)	−0.016 (8)	−0.006 (4)	−0.007 (6)
C63Z	0.083 (6)	0.155 (10)	0.16 (2)	−0.009 (6)	−0.037 (11)	0.092 (12)

Geometric parameters (Å, º) top

Nb1—C3	2.084 (4)	C40—C45	1.398 (6)
Nb1—C4	2.110 (4)	C40—C41	1.412 (6)
Nb1—C5	2.124 (4)	C41—C42	1.401 (7)
Nb1—C6	2.157 (4)	C41—C46	1.497 (7)
Nb1—C7Z	2.233 (6)	C42—C43	1.378 (7)
Nb1—C7"	2.234 (5)	C42—H42	0.9500
Nb1—C7'	2.234 (6)	C43—C44	1.368 (7)
Nb1—C7	2.234 (6)	C43—H43	0.9500
Nb1—N1	2.333 (3)	C44—C45	1.384 (6)
Nb1—N2	2.354 (3)	C44—H44	0.9500
N1—C1	1.312 (4)	C45—C47	1.502 (6)
N1—C8'	1.441 (7)	C46—H46A	0.9800
N1—C8	1.454 (8)	C46—H46B	0.9800
N2—C2	1.312 (4)	C46—H46C	0.9800
N2—C16	1.439 (5)	C47—H47A	0.9800
N3—C3	1.187 (5)	C47—H47B	0.9800
N3—C24	1.393 (5)	C47—H47C	0.9800
N4—C4	1.177 (5)	C48—C53	1.391 (6)
N4—C32	1.388 (5)	C48—C49	1.392 (5)
N5—C5	1.174 (5)	C49—C50	1.389 (6)
N5—C40	1.391 (5)	C49—C54	1.500 (6)
N6—C6	1.174 (5)	C50—C51	1.380 (6)
N6—C48	1.396 (5)	C50—H50	0.9500
C1—C2	1.438 (5)	C51—C52	1.361 (6)
C1—C2ⁱ	1.463 (5)	C51—H51	0.9500
C8—C9	1.409 (12)	C52—C53	1.386 (6)
C8—C13	1.417 (11)	C52—H52	0.9500
C9—C10	1.410 (12)	C53—C55	1.504 (7)
C9—C14	1.497 (9)	C54—H54A	0.9800
C10—C11	1.404 (12)	C54—H54B	0.9800
C10—H10	0.9500	C54—H54C	0.9800
C11—C12	1.403 (13)	C55—H55A	0.9800
C11—H11	0.9500	C55—H55B	0.9800
C12—C13	1.402 (12)	C55—H55C	0.9800
C12—H12	0.9500	C7—N7	1.19 (2)
C13—C15	1.498 (9)	N7—C56	1.454 (16)
C14—H14A	0.9800	C56—C61	1.402 (15)
C14—H14B	0.9800	C56—C57	1.406 (15)
C14—H14C	0.9800	C57—C58	1.422 (16)
C15—H15A	0.9800	C57—C62	1.516 (17)
C15—H15B	0.9800	C58—C59	1.395 (17)
C15—H15C	0.9800	C58—H58	0.9500
C8'—C9'	1.387 (10)	C59—C60	1.394 (17)
C8'—C13'	1.405 (10)	C59—H59	0.9500
C9'—C10'	1.414 (10)	C60—C61	1.420 (16)
C9'—C14'	1.501 (8)	C60—H60	0.9500
C10'—C11'	1.391 (11)	C61—C63	1.513 (18)
C10'—H10'	0.9500	C62—H62A	0.9800
C11'—C12'	1.388 (11)	C62—H62B	0.9800
C11'—H11'	0.9500	C62—H62C	0.9800
C12'—C13'	1.395 (10)	C63—H63A	0.9800
C12'—H12'	0.9500	C63—H63B	0.9800
C13'—C15'	1.495 (8)	C63—H63C	0.9800
C14'—H14D	0.9800	C7'—N7'	1.19 (2)
C14'—H14E	0.9800	N7'—C56'	1.461 (12)
C14'—H14F	0.9800	C56'—C61'	1.402 (13)
C15'—H15D	0.9800	C56'—C57'	1.404 (13)
C15'—H15E	0.9800	C57'—C58'	1.418 (14)
C15'—H15F	0.9800	C57'—C62'	1.524 (15)
C16—C17	1.390 (6)	C58'—C59'	1.391 (14)
C16—C21	1.401 (6)	C58'—H58'	0.9500
C17—C18	1.406 (6)	C59'—C60'	1.398 (14)
C17—C22	1.498 (6)	C59'—H59'	0.9500
C18—C19	1.388 (7)	C60'—C61'	1.421 (14)
C18—H18	0.9500	C60'—H60'	0.9500
C19—C20	1.336 (7)	C61'—C63'	1.502 (15)
C19—H19	0.9500	C62'—H62D	0.9800
C20—C21	1.396 (6)	C62'—H62E	0.9800
C20—H20	0.9500	C62'—H62F	0.9800
C21—C23	1.487 (7)	C63'—H63D	0.9800
C22—H22A	0.9800	C63'—H63E	0.9800
C22—H22B	0.9800	C63'—H63F	0.9800
C22—H22C	0.9800	C7"—N7"	1.18 (2)
C23—H23A	0.9800	N7"—C56"	1.450 (11)
C23—H23B	0.9800	C56"—C57"	1.404 (11)
C23—H23C	0.9800	C56"—C61"	1.409 (12)
C24—C25	1.382 (6)	C57"—C58"	1.407 (12)
C24—C29	1.395 (6)	C57"—C62"	1.533 (13)
C25—C26	1.382 (6)	C58"—C59"	1.401 (13)
C25—C30	1.516 (7)	C58"—H58"	0.9500
C26—C27	1.371 (8)	C59"—C60"	1.391 (13)
C26—H26	0.9500	C59"—H59"	0.9500
C27—C28	1.372 (8)	C60"—C61"	1.422 (13)
C27—H27	0.9500	C60"—H60"	0.9500
C28—C29	1.414 (7)	C61"—C63"	1.508 (14)
C28—H28	0.9500	C62"—H62G	0.9800
C29—C31	1.512 (7)	C62"—H62H	0.9800
C30—H30A	0.9800	C62"—H62I	0.9800
C30—H30B	0.9800	C63"—H63G	0.9800
C30—H30C	0.9800	C63"—H63H	0.9800
C31—H31A	0.9800	C63"—H63I	0.9800
C31—H31B	0.9800	C7Z—N7Z	1.18 (2)
C31—H31C	0.9800	N7Z—C56Z	1.428 (14)
C32—C33	1.382 (6)	C56Z—C61Z	1.401 (14)
C32—C37	1.399 (6)	C56Z—C57Z	1.402 (14)
C33—C34	1.390 (6)	C57Z—C58Z	1.425 (15)
C33—C38	1.504 (6)	C57Z—C62Z	1.522 (16)
C34—C35	1.370 (7)	C58Z—C59Z	1.402 (16)
C34—H34	0.9500	C58Z—H58Z	0.9500
C35—C36	1.362 (6)	C59Z—C60Z	1.397 (16)
C35—H35	0.9500	C59Z—H59Z	0.9500
C36—C37	1.381 (6)	C60Z—C61Z	1.412 (15)
C36—H36	0.9500	C60Z—H60Z	0.9500
C37—C39	1.500 (6)	C61Z—C63Z	1.511 (16)
C38—H38A	0.9800	C62Z—H62J	0.9800
C38—H38B	0.9800	C62Z—H62K	0.9800
C38—H38C	0.9800	C62Z—H62L	0.9800
C39—H39A	0.9800	C63Z—H63J	0.9800
C39—H39B	0.9800	C63Z—H63K	0.9800
C39—H39C	0.9800	C63Z—H63L	0.9800

C3—Nb1—C4	70.68 (15)	C33—C38—H38B	109.5
C3—Nb1—C5	70.12 (14)	H38A—C38—H38B	109.5
C4—Nb1—C5	115.18 (14)	C33—C38—H38C	109.5
C3—Nb1—C6	107.88 (14)	H38A—C38—H38C	109.5
C4—Nb1—C6	72.34 (14)	H38B—C38—H38C	109.5
C5—Nb1—C6	73.36 (15)	C37—C39—H39A	109.5
C3—Nb1—C7Z	78.3 (15)	C37—C39—H39B	109.5
C4—Nb1—C7Z	109 (3)	H39A—C39—H39B	109.5
C5—Nb1—C7Z	111 (2)	C37—C39—H39C	109.5
C6—Nb1—C7Z	173.7 (15)	H39A—C39—H39C	109.5
C3—Nb1—C7"	72 (2)	H39B—C39—H39C	109.5
C4—Nb1—C7"	104.9 (14)	N5—C40—C45	118.7 (4)
C5—Nb1—C7"	109.4 (19)	N5—C40—C41	118.2 (4)
C6—Nb1—C7"	176.9 (14)	C45—C40—C41	123.0 (4)
C3—Nb1—C7'	75 (2)	C42—C41—C40	116.4 (5)
C4—Nb1—C7'	106.5 (18)	C42—C41—C46	122.8 (5)
C5—Nb1—C7'	111 (2)	C40—C41—C46	120.8 (4)
C6—Nb1—C7'	176 (2)	C43—C42—C41	120.4 (5)
C3—Nb1—C7	70 (6)	C43—C42—H42	119.8
C4—Nb1—C7	103 (4)	C41—C42—H42	119.8
C5—Nb1—C7	109 (3)	C44—C43—C42	121.9 (5)
C6—Nb1—C7	175 (4)	C44—C43—H43	119.1
C3—Nb1—N1	135.91 (13)	C42—C43—H43	119.1
C4—Nb1—N1	153.39 (13)	C43—C44—C45	120.5 (5)
C5—Nb1—N1	81.83 (12)	C43—C44—H44	119.7
C6—Nb1—N1	95.14 (13)	C45—C44—H44	119.7
C7Z—Nb1—N1	81 (2)	C44—C45—C40	117.7 (5)
C7"—Nb1—N1	86.8 (17)	C44—C45—C47	121.4 (5)
C7'—Nb1—N1	84.2 (19)	C40—C45—C47	120.9 (4)
C7—Nb1—N1	89 (6)	C41—C46—H46A	109.5
C3—Nb1—N2	135.25 (13)	C41—C46—H46B	109.5
C4—Nb1—N2	81.27 (12)	H46A—C46—H46B	109.5
C5—Nb1—N2	154.60 (13)	C41—C46—H46C	109.5
C6—Nb1—N2	95.30 (13)	H46A—C46—H46C	109.5
C7Z—Nb1—N2	79.1 (18)	H46B—C46—H46C	109.5
C7"—Nb1—N2	83 (2)	C45—C47—H47A	109.5
C7'—Nb1—N2	80 (2)	C45—C47—H47B	109.5
C7—Nb1—N2	84 (5)	H47A—C47—H47B	109.5
N1—Nb1—N2	76.54 (10)	C45—C47—H47C	109.5
C1—N1—C8'	122.2 (9)	H47A—C47—H47C	109.5
C1—N1—C8	117.3 (12)	H47B—C47—H47C	109.5
C1—N1—Nb1	108.3 (2)	C53—C48—C49	123.0 (4)
C8'—N1—Nb1	128.9 (9)	C53—C48—N6	119.2 (4)
C8—N1—Nb1	126.0 (13)	C49—C48—N6	117.8 (4)
C2—N2—C16	119.0 (3)	C50—C49—C48	116.8 (4)
C2—N2—Nb1	107.3 (2)	C50—C49—C54	121.9 (4)
C16—N2—Nb1	131.0 (2)	C48—C49—C54	121.3 (4)
C3—N3—C24	171.1 (5)	C51—C50—C49	121.2 (4)
C4—N4—C32	175.2 (4)	C51—C50—H50	119.4
C5—N5—C40	173.6 (4)	C49—C50—H50	119.4
C6—N6—C48	163.3 (4)	C52—C51—C50	120.4 (4)
N1—C1—C2	123.6 (3)	C52—C51—H51	119.8
N1—C1—C2ⁱ	146.5 (3)	C50—C51—H51	119.8
C2—C1—C2ⁱ	90.0 (3)	C51—C52—C53	121.1 (5)
N2—C2—C1	124.3 (3)	C51—C52—H52	119.4
N2—C2—C1ⁱ	145.7 (3)	C53—C52—H52	119.4
C1—C2—C1ⁱ	90.0 (3)	C52—C53—C48	117.5 (4)
N3—C3—Nb1	177.4 (4)	C52—C53—C55	121.9 (5)
N4—C4—Nb1	176.2 (3)	C48—C53—C55	120.6 (4)
N5—C5—Nb1	175.3 (4)	C49—C54—H54A	109.5
N6—C6—Nb1	174.4 (3)	C49—C54—H54B	109.5
C9—C8—C13	118.7 (9)	H54A—C54—H54B	109.5
C9—C8—N1	126.8 (11)	C49—C54—H54C	109.5
C13—C8—N1	114.5 (11)	H54A—C54—H54C	109.5
C8—C9—C10	118.9 (12)	H54B—C54—H54C	109.5
C8—C9—C14	120 (2)	C53—C55—H55A	109.5
C10—C9—C14	120.8 (19)	C53—C55—H55B	109.5
C11—C10—C9	121.3 (12)	H55A—C55—H55B	109.5
C11—C10—H10	119.3	C53—C55—H55C	109.5
C9—C10—H10	119.3	H55A—C55—H55C	109.5
C12—C11—C10	120.5 (12)	H55B—C55—H55C	109.5
C12—C11—H11	119.7	N7—C7—Nb1	164 (6)
C10—C11—H11	119.7	C7—N7—C56	155 (7)
C13—C12—C11	117.9 (12)	C61—C56—C57	122.5 (19)
C13—C12—H12	121.1	C61—C56—N7	120 (2)
C11—C12—H12	121.1	C57—C56—N7	117.9 (19)
C12—C13—C8	122.6 (10)	C56—C57—C58	117.3 (19)
C12—C13—C15	116.9 (14)	C56—C57—C62	132 (4)
C8—C13—C15	120.5 (14)	C58—C57—C62	111 (4)
C9—C14—H14A	109.5	C59—C58—C57	123 (2)
C9—C14—H14B	109.5	C59—C58—H58	118.6
H14A—C14—H14B	109.5	C57—C58—H58	118.6
C9—C14—H14C	109.5	C60—C59—C58	117 (2)
H14A—C14—H14C	109.5	C60—C59—H59	121.5
H14B—C14—H14C	109.5	C58—C59—H59	121.5
C13—C15—H15A	109.5	C59—C60—C61	124 (2)
C13—C15—H15B	109.5	C59—C60—H60	118.2
H15A—C15—H15B	109.5	C61—C60—H60	118.2
C13—C15—H15C	109.5	C56—C61—C60	116.8 (19)
H15A—C15—H15C	109.5	C56—C61—C63	122 (7)
H15B—C15—H15C	109.5	C60—C61—C63	121 (7)
C9'—C8'—C13'	124.8 (7)	C57—C62—H62A	109.5
C9'—C8'—N1	113.9 (7)	C57—C62—H62B	109.5
C13'—C8'—N1	120.8 (8)	H62A—C62—H62B	109.5
C8'—C9'—C10'	117.0 (8)	C57—C62—H62C	109.5
C8'—C9'—C14'	124.0 (13)	H62A—C62—H62C	109.5
C10'—C9'—C14'	118.9 (12)	H62B—C62—H62C	109.5
C11'—C10'—C9'	119.1 (10)	C61—C63—H63A	109.5
C11'—C10'—H10'	120.4	C61—C63—H63B	109.5
C9'—C10'—H10'	120.4	H63A—C63—H63B	109.5
C12'—C11'—C10'	122.4 (10)	C61—C63—H63C	109.5
C12'—C11'—H11'	118.8	H63A—C63—H63C	109.5
C10'—C11'—H11'	118.8	H63B—C63—H63C	109.5
C11'—C12'—C13'	120.0 (9)	N7'—C7'—Nb1	165 (6)
C11'—C12'—H12'	120.0	C7'—N7'—C56'	157 (4)
C13'—C12'—H12'	120.0	C61'—C56'—C57'	122.4 (13)
C12'—C13'—C8'	116.7 (8)	C61'—C56'—N7'	119.3 (14)
C12'—C13'—C15'	121.3 (9)	C57'—C56'—N7'	118.3 (14)
C8'—C13'—C15'	121.9 (9)	C56'—C57'—C58'	116.4 (14)
C9'—C14'—H14D	109.5	C56'—C57'—C62'	112.9 (19)
C9'—C14'—H14E	109.5	C58'—C57'—C62'	131 (2)
H14D—C14'—H14E	109.5	C59'—C58'—C57'	124.0 (15)
C9'—C14'—H14F	109.5	C59'—C58'—H58'	118.0
H14D—C14'—H14F	109.5	C57'—C58'—H58'	118.0
H14E—C14'—H14F	109.5	C58'—C59'—C60'	117.2 (15)
C13'—C15'—H15D	109.5	C58'—C59'—H59'	121.4
C13'—C15'—H15E	109.5	C60'—C59'—H59'	121.4
H15D—C15'—H15E	109.5	C59'—C60'—C61'	121.9 (14)
C13'—C15'—H15F	109.5	C59'—C60'—H60'	119.0
H15D—C15'—H15F	109.5	C61'—C60'—H60'	119.0
H15E—C15'—H15F	109.5	C56'—C61'—C60'	118.1 (13)
C17—C16—C21	120.9 (4)	C56'—C61'—C63'	119 (2)
C17—C16—N2	119.7 (4)	C60'—C61'—C63'	123 (2)
C21—C16—N2	119.2 (4)	C57'—C62'—H62D	109.5
C16—C17—C18	118.0 (5)	C57'—C62'—H62E	109.5
C16—C17—C22	121.3 (4)	H62D—C62'—H62E	109.5
C18—C17—C22	120.7 (5)	C57'—C62'—H62F	109.5
C19—C18—C17	120.8 (5)	H62D—C62'—H62F	109.5
C19—C18—H18	119.6	H62E—C62'—H62F	109.5
C17—C18—H18	119.6	C61'—C63'—H63D	109.5
C20—C19—C18	119.9 (5)	C61'—C63'—H63E	109.5
C20—C19—H19	120.0	H63D—C63'—H63E	109.5
C18—C19—H19	120.0	C61'—C63'—H63F	109.5
C19—C20—C21	122.1 (5)	H63D—C63'—H63F	109.5
C19—C20—H20	119.0	H63E—C63'—H63F	109.5
C21—C20—H20	119.0	N7"—C7"—Nb1	166 (6)
C20—C21—C16	118.2 (5)	C7"—N7"—C56"	159 (5)
C20—C21—C23	120.0 (5)	C57"—C56"—C61"	124.3 (10)
C16—C21—C23	121.8 (4)	C57"—C56"—N7"	117.6 (11)
C17—C22—H22A	109.5	C61"—C56"—N7"	118.1 (11)
C17—C22—H22B	109.5	C56"—C57"—C58"	116.4 (11)
H22A—C22—H22B	109.5	C56"—C57"—C62"	129.3 (15)
C17—C22—H22C	109.5	C58"—C57"—C62"	114.3 (16)
H22A—C22—H22C	109.5	C59"—C58"—C57"	122.1 (12)
H22B—C22—H22C	109.5	C59"—C58"—H58"	118.9
C21—C23—H23A	109.5	C57"—C58"—H58"	118.9
C21—C23—H23B	109.5	C60"—C59"—C58"	119.3 (12)
H23A—C23—H23B	109.5	C60"—C59"—H59"	120.4
C21—C23—H23C	109.5	C58"—C59"—H59"	120.4
H23A—C23—H23C	109.5	C59"—C60"—C61"	121.8 (12)
H23B—C23—H23C	109.5	C59"—C60"—H60"	119.1
C25—C24—N3	119.1 (4)	C61"—C60"—H60"	119.1
C25—C24—C29	123.3 (4)	C56"—C61"—C60"	116.1 (11)
N3—C24—C29	117.6 (5)	C56"—C61"—C63"	122.4 (16)
C26—C25—C24	118.0 (5)	C60"—C61"—C63"	121.4 (17)
C26—C25—C30	119.3 (5)	C57"—C62"—H62G	109.5
C24—C25—C30	122.7 (4)	C57"—C62"—H62H	109.5
C27—C26—C25	120.7 (6)	H62G—C62"—H62H	109.5
C27—C26—H26	119.7	C57"—C62"—H62I	109.5
C25—C26—H26	119.7	H62G—C62"—H62I	109.5
C26—C27—C28	121.2 (5)	H62H—C62"—H62I	109.5
C26—C27—H27	119.4	C61"—C63"—H63G	109.5
C28—C27—H27	119.4	C61"—C63"—H63H	109.5
C27—C28—C29	120.3 (5)	H63G—C63"—H63H	109.5
C27—C28—H28	119.8	C61"—C63"—H63I	109.5
C29—C28—H28	119.8	H63G—C63"—H63I	109.5
C24—C29—C28	116.5 (5)	H63H—C63"—H63I	109.5
C24—C29—C31	122.1 (4)	N7Z—C7Z—Nb1	162 (5)
C28—C29—C31	121.4 (5)	C7Z—N7Z—C56Z	163 (4)
C25—C30—H30A	109.5	C61Z—C56Z—C57Z	125.3 (15)
C25—C30—H30B	109.5	C61Z—C56Z—N7Z	114.2 (15)
H30A—C30—H30B	109.5	C57Z—C56Z—N7Z	120.5 (16)
C25—C30—H30C	109.5	C56Z—C57Z—C58Z	114.1 (15)
H30A—C30—H30C	109.5	C56Z—C57Z—C62Z	122 (2)
H30B—C30—H30C	109.5	C58Z—C57Z—C62Z	124 (3)
C29—C31—H31A	109.5	C59Z—C58Z—C57Z	123.5 (18)
C29—C31—H31B	109.5	C59Z—C58Z—H58Z	118.3
H31A—C31—H31B	109.5	C57Z—C58Z—H58Z	118.3
C29—C31—H31C	109.5	C60Z—C59Z—C58Z	118.8 (19)
H31A—C31—H31C	109.5	C60Z—C59Z—H59Z	120.6
H31B—C31—H31C	109.5	C58Z—C59Z—H59Z	120.6
C33—C32—N4	117.7 (4)	C59Z—C60Z—C61Z	120.9 (17)
C33—C32—C37	123.3 (4)	C59Z—C60Z—H60Z	119.5
N4—C32—C37	119.0 (4)	C61Z—C60Z—H60Z	119.5
C32—C33—C34	116.4 (4)	C56Z—C61Z—C60Z	117.3 (16)
C32—C33—C38	121.3 (4)	C56Z—C61Z—C63Z	122.3 (19)
C34—C33—C38	122.3 (4)	C60Z—C61Z—C63Z	120 (2)
C35—C34—C33	121.4 (5)	C57Z—C62Z—H62J	109.5
C35—C34—H34	119.3	C57Z—C62Z—H62K	109.5
C33—C34—H34	119.3	H62J—C62Z—H62K	109.5
C36—C35—C34	120.7 (4)	C57Z—C62Z—H62L	109.5
C36—C35—H35	119.7	H62J—C62Z—H62L	109.5
C34—C35—H35	119.7	H62K—C62Z—H62L	109.5
C35—C36—C37	120.9 (4)	C61Z—C63Z—H63J	109.5
C35—C36—H36	119.6	C61Z—C63Z—H63K	109.5
C37—C36—H36	119.6	H63J—C63Z—H63K	109.5
C36—C37—C32	117.2 (4)	C61Z—C63Z—H63L	109.5
C36—C37—C39	121.7 (4)	H63J—C63Z—H63L	109.5
C32—C37—C39	121.0 (4)	H63K—C63Z—H63L	109.5
C33—C38—H38A	109.5

C8'—N1—C1—C2	172.2 (6)	C45—C40—C41—C42	2.8 (6)
C8—N1—C1—C2	150.3 (9)	N5—C40—C41—C46	0.6 (6)
Nb1—N1—C1—C2	0.1 (5)	C45—C40—C41—C46	179.8 (4)
C8'—N1—C1—C2ⁱ	−5.5 (9)	C40—C41—C42—C43	−3.0 (7)
C8—N1—C1—C2ⁱ	−27.5 (11)	C46—C41—C42—C43	−180.0 (5)
Nb1—N1—C1—C2ⁱ	−177.7 (5)	C41—C42—C43—C44	2.6 (9)
C16—N2—C2—C1	−163.4 (4)	C42—C43—C44—C45	−1.7 (9)
Nb1—N2—C2—C1	−0.2 (4)	C43—C44—C45—C40	1.3 (7)
C16—N2—C2—C1ⁱ	14.5 (8)	C43—C44—C45—C47	178.8 (5)
Nb1—N2—C2—C1ⁱ	177.8 (5)	N5—C40—C45—C44	177.2 (4)
N1—C1—C2—N2	0.1 (6)	C41—C40—C45—C44	−2.0 (6)
C2ⁱ—C1—C2—N2	178.8 (5)	N5—C40—C45—C47	−0.3 (6)
N1—C1—C2—C1ⁱ	−178.8 (5)	C41—C40—C45—C47	−179.5 (4)
C2ⁱ—C1—C2—C1ⁱ	−0.001 (1)	C6—N6—C48—C49	1.5 (16)
C1—N1—C8—C9	−56 (3)	C53—C48—C49—C50	0.4 (7)
Nb1—N1—C8—C9	89 (3)	N6—C48—C49—C50	180.0 (4)
C1—N1—C8—C13	126.1 (19)	C53—C48—C49—C54	−177.5 (4)
Nb1—N1—C8—C13	−90 (2)	N6—C48—C49—C54	2.1 (6)
C13—C8—C9—C10	0 (4)	C48—C49—C50—C51	0.9 (7)
N1—C8—C9—C10	−178 (2)	C54—C49—C50—C51	178.8 (4)
C13—C8—C9—C14	−177 (3)	C49—C50—C51—C52	−1.9 (8)
N1—C8—C9—C14	5 (5)	C50—C51—C52—C53	1.5 (8)
C8—C9—C10—C11	1 (4)	C51—C52—C53—C48	−0.2 (8)
C14—C9—C10—C11	178 (3)	C51—C52—C53—C55	179.9 (5)
C9—C10—C11—C12	−1 (4)	C49—C48—C53—C52	−0.8 (7)
C10—C11—C12—C13	−1 (4)	N6—C48—C53—C52	179.7 (4)
C11—C12—C13—C8	3 (4)	C49—C48—C53—C55	179.1 (5)
C11—C12—C13—C15	−177 (2)	N6—C48—C53—C55	−0.4 (7)
C9—C8—C13—C12	−2 (4)	Nb1—C7—N7—C56	−50 (80)
N1—C8—C13—C12	177 (2)	C7—N7—C56—C61	−84 (23)
C9—C8—C13—C15	178 (2)	C7—N7—C56—C57	96 (23)
N1—C8—C13—C15	−4 (3)	C61—C56—C57—C58	0.1 (8)
C1—N1—C8'—C9'	−72.0 (18)	N7—C56—C57—C58	180.0 (5)
Nb1—N1—C8'—C9'	98.5 (17)	C61—C56—C57—C62	−180.0 (8)
C1—N1—C8'—C13'	116.0 (15)	N7—C56—C57—C62	−0.1 (6)
Nb1—N1—C8'—C13'	−73.6 (17)	C56—C57—C58—C59	0.1 (12)
C13'—C8'—C9'—C10'	−2 (3)	C62—C57—C58—C59	−179.8 (10)
N1—C8'—C9'—C10'	−173.6 (15)	C57—C58—C59—C60	−0.2 (16)
C13'—C8'—C9'—C14'	175 (2)	C58—C59—C60—C61	0.0 (17)
N1—C8'—C9'—C14'	3 (3)	C57—C56—C61—C60	−0.2 (12)
C8'—C9'—C10'—C11'	0 (3)	N7—C56—C61—C60	179.9 (7)
C14'—C9'—C10'—C11'	−177.1 (18)	C57—C56—C61—C63	−179.9 (7)
C9'—C10'—C11'—C12'	1 (2)	N7—C56—C61—C63	0.2 (12)
C10'—C11'—C12'—C13'	−1 (2)	C59—C60—C61—C56	0.2 (16)
C11'—C12'—C13'—C8'	−1 (2)	C59—C60—C61—C63	179.8 (11)
C11'—C12'—C13'—C15'	−178.2 (13)	Nb1—C7'—N7'—C56'	−100 (26)
C9'—C8'—C13'—C12'	2 (3)	C7'—N7'—C56'—C61'	−97 (11)
N1—C8'—C13'—C12'	173.3 (14)	C7'—N7'—C56'—C57'	83 (11)
C9'—C8'—C13'—C15'	179.7 (18)	C61'—C56'—C57'—C58'	−0.2 (7)
N1—C8'—C13'—C15'	−9 (3)	N7'—C56'—C57'—C58'	179.8 (5)
C2—N2—C16—C17	65.8 (5)	C61'—C56'—C57'—C62'	179.6 (7)
Nb1—N2—C16—C17	−92.8 (4)	N7'—C56'—C57'—C62'	−0.3 (5)
C2—N2—C16—C21	−118.9 (4)	C56'—C57'—C58'—C59'	0.6 (12)
Nb1—N2—C16—C21	82.5 (4)	C62'—C57'—C58'—C59'	−179.3 (9)
C21—C16—C17—C18	1.9 (6)	C57'—C58'—C59'—C60'	−0.9 (15)
N2—C16—C17—C18	177.1 (4)	C58'—C59'—C60'—C61'	0.9 (16)
C21—C16—C17—C22	−176.9 (4)	C57'—C56'—C61'—C60'	0.3 (11)
N2—C16—C17—C22	−1.7 (6)	N7'—C56'—C61'—C60'	−179.8 (7)
C16—C17—C18—C19	−0.4 (7)	C57'—C56'—C61'—C63'	−179.9 (6)
C22—C17—C18—C19	178.4 (4)	N7'—C56'—C61'—C63'	0.1 (11)
C17—C18—C19—C20	−1.4 (8)	C59'—C60'—C61'—C56'	−0.7 (15)
C18—C19—C20—C21	1.7 (8)	C59'—C60'—C61'—C63'	179.5 (10)
C19—C20—C21—C16	−0.2 (7)	Nb1—C7"—N7"—C56"	134 (21)
C19—C20—C21—C23	−179.4 (5)	C7"—N7"—C56"—C57"	−52 (8)
C17—C16—C21—C20	−1.7 (6)	C7"—N7"—C56"—C61"	128 (8)
N2—C16—C21—C20	−176.9 (4)	C61"—C56"—C57"—C58"	−0.2 (7)
C17—C16—C21—C23	177.6 (4)	N7"—C56"—C57"—C58"	179.8 (5)
N2—C16—C21—C23	2.4 (6)	C61"—C56"—C57"—C62"	179.8 (7)
N3—C24—C25—C26	179.7 (4)	N7"—C56"—C57"—C62"	−0.3 (5)
C29—C24—C25—C26	−1.2 (7)	C56"—C57"—C58"—C59"	0.6 (11)
N3—C24—C25—C30	1.3 (7)	C62"—C57"—C58"—C59"	−179.4 (9)
C29—C24—C25—C30	−179.6 (4)	C57"—C58"—C59"—C60"	−0.8 (15)
C24—C25—C26—C27	0.3 (7)	C58"—C59"—C60"—C61"	0.7 (16)
C30—C25—C26—C27	178.8 (5)	C57"—C56"—C61"—C60"	0.0 (11)
C25—C26—C27—C28	−0.1 (8)	N7"—C56"—C61"—C60"	−179.9 (7)
C26—C27—C28—C29	0.6 (8)	C57"—C56"—C61"—C63"	−179.8 (7)
C25—C24—C29—C28	1.7 (7)	N7"—C56"—C61"—C63"	0.2 (11)
N3—C24—C29—C28	−179.2 (4)	C59"—C60"—C61"—C56"	−0.2 (14)
C25—C24—C29—C31	−176.7 (4)	C59"—C60"—C61"—C63"	179.6 (10)
N3—C24—C29—C31	2.5 (6)	Nb1—C7Z—N7Z—C56Z	−61 (36)
C27—C28—C29—C24	−1.4 (7)	C7Z—N7Z—C56Z—C61Z	148 (15)
C27—C28—C29—C31	177.0 (5)	C7Z—N7Z—C56Z—C57Z	−32 (15)
N4—C32—C33—C34	−178.0 (4)	C61Z—C56Z—C57Z—C58Z	0.3 (8)
C37—C32—C33—C34	1.8 (7)	N7Z—C56Z—C57Z—C58Z	−179.9 (5)
N4—C32—C33—C38	3.8 (6)	C61Z—C56Z—C57Z—C62Z	−179.9 (8)
C37—C32—C33—C38	−176.3 (4)	N7Z—C56Z—C57Z—C62Z	−0.1 (5)
C32—C33—C34—C35	−0.9 (8)	C56Z—C57Z—C58Z—C59Z	−0.1 (13)
C38—C33—C34—C35	177.2 (5)	C62Z—C57Z—C58Z—C59Z	−179.9 (10)
C33—C34—C35—C36	−1.2 (9)	C57Z—C58Z—C59Z—C60Z	−0.3 (17)
C34—C35—C36—C37	2.5 (8)	C58Z—C59Z—C60Z—C61Z	0.6 (17)
C35—C36—C37—C32	−1.6 (7)	C57Z—C56Z—C61Z—C60Z	0.0 (12)
C35—C36—C37—C39	−179.2 (5)	N7Z—C56Z—C61Z—C60Z	−179.8 (8)
C33—C32—C37—C36	−0.6 (6)	C57Z—C56Z—C61Z—C63Z	−179.3 (7)
N4—C32—C37—C36	179.2 (4)	N7Z—C56Z—C61Z—C63Z	0.8 (12)
C33—C32—C37—C39	177.0 (4)	C59Z—C60Z—C61Z—C56Z	−0.5 (16)
N4—C32—C37—C39	−3.1 (6)	C59Z—C60Z—C61Z—C63Z	178.9 (11)
N5—C40—C41—C42	−176.4 (4)

Symmetry code: (i) −x, −y+1, −z+2.

Bis[µ-N,N',N'',N'''-tetrakis(2,6-\ dimethylphenyl)squaramidinato(2-)]bis[tetrakis(2,6-dimethylphenyl isocyanide)niobium(I)] tetrahydrofuran trisolvate (2) top

Crystal data top

[Nb₂(C₉H₉N)₈(C₃₆H₃₆N₄)]·3C₄H₈O	Z = 1
M_r = 1976.19	F(000) = 1042
Triclinic, P1	D_x = 1.231 Mg m⁻³
a = 12.2029 (13) Å	Mo Kα radiation, λ = 0.71073 Å
b = 12.5921 (14) Å	Cell parameters from 2821 reflections
c = 19.676 (2) Å	θ = 1.1–25.1°
α = 95.620 (2)°	µ = 0.27 mm⁻¹
β = 101.807 (2)°	T = 173 K
γ = 113.236 (2)°	Rod, black
V = 2665.2 (5) Å³	0.40 × 0.20 × 0.10 mm

Data collection top

Bruker SMART CCD platform diffractometer	6686 reflections with I > 2σ(I)
Radiation source: normal-focus sealed tube	R_int = 0.040
ω scans	θ_max = 25.1°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→14
T_min = 0.899, T_max = 0.973	k = −14→15
18395 measured reflections	l = −18→23
9307 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)] = 0.048	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.107	H-atom parameters constrained
S = 1.02	w = 1/[σ²(F_o²) + (0.0421P)² + 1.0933P] where P = (F_o² + 2F_c²)/3
9307 reflections	(Δ/σ)_max = 0.001
680 parameters	Δρ_max = 0.39 e Å⁻³
58 restraints	Δρ_min = −0.36 e Å⁻³

Special details top

Refinement. THF solvent molecule O1/C55-C58 is modeled as disordered over two positions, 0.536 (8):0.464 (8). THF solvent molecule O2/C59-C62 was modeled as disordered over a crystallographic inversion center (0.50:0.50).

Analogous bond lengths and angles were restrained to be similar and anisotropic displacement parameters for pairs of proximal and symmetry-related atoms were restrained to be similar or constrained to be equivalent. O–C andC–C bond lengths for THF molecule O1/C55-C58 were restrained toward ideal values.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Nb1	0.57320 (3)	0.50730 (3)	0.68770 (2)	0.02883 (10)
N1	0.6605 (2)	0.5876 (2)	0.60352 (13)	0.0295 (6)
N2	0.4103 (2)	0.4358 (2)	0.59059 (13)	0.0297 (6)
N3	0.5491 (3)	0.6757 (3)	0.81385 (16)	0.0446 (8)
N4	0.3673 (3)	0.3418 (3)	0.76245 (15)	0.0444 (8)
N5	0.6764 (3)	0.3225 (3)	0.74646 (16)	0.0510 (8)
N6	0.8486 (3)	0.6647 (3)	0.79647 (15)	0.0456 (8)
C1	0.5776 (3)	0.5429 (3)	0.54152 (15)	0.0254 (7)
C2	0.4498 (3)	0.4657 (3)	0.53506 (15)	0.0268 (7)
C3	0.5587 (3)	0.6129 (3)	0.76794 (17)	0.0352 (8)
C4	0.4421 (3)	0.4001 (3)	0.73619 (17)	0.0347 (8)
C5	0.6378 (3)	0.3903 (3)	0.72580 (17)	0.0385 (8)
C6	0.7515 (3)	0.6063 (3)	0.75656 (18)	0.0363 (8)
C7	0.7869 (3)	0.6632 (3)	0.60681 (16)	0.0378 (9)
C8	0.8335 (4)	0.7828 (3)	0.6365 (2)	0.0569 (11)
C9	0.9574 (5)	0.8546 (4)	0.6403 (3)	0.0862 (17)
H9	0.992079	0.936200	0.660757	0.103*
C10	1.0280 (5)	0.8088 (7)	0.6151 (3)	0.104 (2)
H10	1.110985	0.859478	0.617251	0.124*
C11	0.9830 (4)	0.6921 (6)	0.5868 (2)	0.0812 (16)
H11	1.034877	0.662390	0.569676	0.097*
C12	0.8608 (3)	0.6153 (4)	0.58274 (19)	0.0525 (10)
C13	0.7558 (5)	0.8335 (4)	0.6645 (2)	0.0789 (15)
H13A	0.677088	0.809232	0.628751	0.118*
H13B	0.799542	0.919718	0.675498	0.118*
H13C	0.739811	0.804739	0.707593	0.118*
C14	0.8127 (4)	0.4862 (4)	0.5568 (2)	0.0665 (12)
H14A	0.879166	0.468004	0.546244	0.100*
H14B	0.744613	0.461262	0.513806	0.100*
H14C	0.782681	0.444310	0.593417	0.100*
C15	0.2847 (3)	0.3561 (3)	0.58493 (16)	0.0371 (8)
C16	0.2457 (4)	0.2356 (3)	0.56130 (19)	0.0510 (10)
C17	0.1253 (4)	0.1590 (4)	0.5613 (2)	0.0770 (15)
H17	0.095909	0.076589	0.545053	0.092*
C18	0.0497 (5)	0.2031 (6)	0.5847 (3)	0.0944 (19)
H18	−0.031676	0.150535	0.584435	0.113*
C19	0.0897 (4)	0.3201 (6)	0.6079 (2)	0.0805 (16)
H19	0.035380	0.348061	0.623455	0.097*
C20	0.2085 (3)	0.4009 (4)	0.60979 (19)	0.0517 (10)
C21	0.3304 (4)	0.1897 (3)	0.5385 (2)	0.0661 (12)
H21A	0.407339	0.217894	0.576354	0.099*
H21B	0.349144	0.217600	0.495652	0.099*
H21C	0.290640	0.103257	0.528514	0.099*
C22	0.2527 (4)	0.5295 (4)	0.6381 (2)	0.0660 (12)
H22A	0.181794	0.546322	0.641083	0.099*
H22B	0.295503	0.575251	0.606402	0.099*
H22C	0.309790	0.551119	0.685381	0.099*
C23	0.5571 (3)	0.7353 (3)	0.87918 (17)	0.0339 (8)
C24	0.5339 (3)	0.8360 (3)	0.88106 (18)	0.0387 (8)
C25	0.5452 (3)	0.8954 (3)	0.94660 (19)	0.0442 (9)
H25	0.531794	0.964881	0.949650	0.053*
C26	0.5754 (3)	0.8568 (3)	1.00783 (19)	0.0453 (9)
H26	0.581791	0.898897	1.052332	0.054*
C27	0.5965 (3)	0.7565 (3)	1.00420 (18)	0.0411 (9)
H27	0.617162	0.730250	1.046584	0.049*
C28	0.5881 (3)	0.6940 (3)	0.94047 (18)	0.0369 (8)
C29	0.4988 (4)	0.8756 (3)	0.8135 (2)	0.0577 (11)
H29A	0.483485	0.945308	0.824362	0.087*
H29B	0.423626	0.811968	0.781776	0.087*
H29C	0.566268	0.895164	0.790449	0.087*
C30	0.6127 (4)	0.5858 (3)	0.9361 (2)	0.0534 (10)
H30A	0.642479	0.575237	0.983976	0.080*
H30B	0.675618	0.595058	0.910257	0.080*
H30C	0.536159	0.516501	0.911080	0.080*
C31	0.2795 (3)	0.2697 (3)	0.79359 (18)	0.0405 (9)
C32	0.2535 (3)	0.1503 (3)	0.78455 (19)	0.0459 (9)
C33	0.1692 (4)	0.0819 (4)	0.8173 (2)	0.0577 (11)
H33	0.149698	0.000160	0.812551	0.069*
C34	0.1128 (4)	0.1295 (4)	0.8568 (2)	0.0677 (13)
H34	0.055126	0.080655	0.878964	0.081*
C35	0.1394 (4)	0.2475 (4)	0.8643 (2)	0.0615 (12)
H35	0.099488	0.278958	0.891688	0.074*
C36	0.2233 (3)	0.3216 (3)	0.8327 (2)	0.0471 (10)
C37	0.3150 (4)	0.0995 (4)	0.7403 (2)	0.0697 (13)
H37A	0.287121	0.015235	0.740820	0.105*
H37B	0.404951	0.140129	0.759837	0.105*
H37C	0.292885	0.110045	0.691488	0.105*
C38	0.2527 (4)	0.4504 (4)	0.8404 (2)	0.0670 (12)
H38A	0.207802	0.470317	0.871784	0.101*
H38B	0.227621	0.467811	0.793821	0.101*
H38C	0.341847	0.497096	0.860745	0.101*
C39	0.7154 (3)	0.2535 (3)	0.78667 (18)	0.0377 (8)
C40	0.7757 (3)	0.1925 (3)	0.7587 (2)	0.0449 (9)
C41	0.8139 (4)	0.1244 (4)	0.7999 (3)	0.0641 (12)
H41	0.854156	0.081246	0.782141	0.077*
C42	0.7945 (4)	0.1179 (4)	0.8662 (3)	0.0712 (13)
H42	0.821010	0.070162	0.893685	0.085*
C43	0.7372 (4)	0.1800 (3)	0.8927 (2)	0.0592 (11)
H43	0.725586	0.175906	0.938814	0.071*
C44	0.6959 (3)	0.2484 (3)	0.85364 (19)	0.0403 (8)
C45	0.7996 (4)	0.2033 (4)	0.6872 (2)	0.0760 (14)
H45A	0.847295	0.159249	0.677853	0.114*
H45B	0.846412	0.286588	0.686422	0.114*
H45C	0.720541	0.171195	0.650770	0.114*
C46	0.6334 (4)	0.3174 (4)	0.8829 (2)	0.0591 (11)
H46A	0.677247	0.400748	0.881206	0.089*
H46B	0.634751	0.309350	0.932048	0.089*
H46C	0.547463	0.286856	0.854383	0.089*
C47	0.9716 (3)	0.7229 (3)	0.83431 (18)	0.0414 (9)
C48	1.0572 (4)	0.6863 (3)	0.8150 (2)	0.0514 (10)
C49	1.1787 (4)	0.7456 (4)	0.8541 (2)	0.0604 (11)
H49	1.238967	0.722581	0.842372	0.073*
C50	1.2141 (4)	0.8368 (4)	0.9095 (2)	0.0651 (13)
H50	1.298684	0.876936	0.935310	0.078*
C51	1.1287 (4)	0.8712 (3)	0.9283 (2)	0.0571 (11)
H51	1.154751	0.934430	0.967231	0.069*
C52	1.0049 (3)	0.8143 (3)	0.89102 (19)	0.0433 (9)
C53	1.0141 (4)	0.5833 (4)	0.7552 (2)	0.0775 (14)
H53A	1.085560	0.571737	0.747093	0.116*
H53B	0.971343	0.598819	0.712114	0.116*
H53C	0.957228	0.512211	0.767356	0.116*
C54	0.9087 (4)	0.8479 (4)	0.9110 (2)	0.0665 (12)
H54A	0.857036	0.856341	0.868500	0.100*
H54B	0.949472	0.922961	0.945171	0.100*
H54C	0.856728	0.786471	0.932214	0.100*
O1	0.3329 (10)	0.9262 (12)	0.5822 (9)	0.159 (5)	0.459 (8)
C55	0.3266 (13)	0.8267 (15)	0.5316 (8)	0.162 (4)	0.459 (8)
H55A	0.342531	0.850229	0.486755	0.194*	0.459 (8)
H55B	0.245591	0.757554	0.521116	0.194*	0.459 (8)
C56	0.4316 (14)	0.8018 (12)	0.5741 (12)	0.155 (6)	0.459 (8)
H56A	0.412392	0.768764	0.616060	0.186*	0.459 (8)
H56B	0.454665	0.749933	0.544519	0.186*	0.459 (8)
C57	0.5240 (11)	0.9230 (13)	0.5928 (11)	0.150 (6)	0.459 (8)
H57A	0.542704	0.955029	0.550451	0.180*	0.459 (8)
H57B	0.601498	0.931819	0.625854	0.180*	0.459 (8)
C58	0.4565 (12)	0.9799 (13)	0.6282 (7)	0.115 (5)	0.459 (8)
H58A	0.457011	0.962861	0.676347	0.137*	0.459 (8)
H58B	0.494215	1.066343	0.631626	0.137*	0.459 (8)
O1'	0.3511 (11)	0.8622 (14)	0.6171 (6)	0.188 (5)	0.541 (8)
C55'	0.3033 (10)	0.8369 (14)	0.5386 (7)	0.162 (4)	0.541 (8)
H55C	0.285441	0.901496	0.521908	0.194*	0.541 (8)
H55D	0.227843	0.761747	0.521509	0.194*	0.541 (8)
C56'	0.4131 (12)	0.8288 (12)	0.5153 (7)	0.117 (4)	0.541 (8)
H56C	0.424924	0.758185	0.525858	0.140*	0.541 (8)
H56D	0.406617	0.831734	0.464606	0.140*	0.541 (8)
C57'	0.5075 (11)	0.9368 (13)	0.5618 (7)	0.169 (6)	0.541 (8)
H57C	0.494687	1.006793	0.551022	0.203*	0.541 (8)
H57D	0.591769	0.947914	0.559954	0.203*	0.541 (8)
C58'	0.4838 (12)	0.9103 (16)	0.6321 (6)	0.153 (6)	0.541 (8)
H58C	0.514679	0.852267	0.647430	0.184*	0.541 (8)
H58D	0.523654	0.982869	0.669219	0.184*	0.541 (8)
O2	−0.1056 (8)	0.5221 (7)	1.0162 (4)	0.096 (2)	0.5
C59	−0.057 (3)	0.562 (3)	0.9627 (16)	0.097 (5)	0.5
H59A	−0.001643	0.646856	0.976764	0.116*	0.5
H59B	−0.124060	0.548958	0.920132	0.116*	0.5
C60	0.012 (4)	0.492 (4)	0.9481 (16)	0.094 (6)	0.5
H60A	0.094461	0.544259	0.942770	0.113*	0.5
H60B	−0.033760	0.431414	0.904173	0.113*	0.5
C61	0.026 (3)	0.436 (3)	1.0113 (15)	0.097 (5)	0.5
H61A	−0.016561	0.348712	0.997454	0.116*	0.5
H61B	0.114778	0.459092	1.034645	0.116*	0.5
C62	−0.032 (4)	0.482 (4)	1.0587 (16)	0.094 (6)	0.5
H62A	−0.082858	0.418872	1.080275	0.113*	0.5
H62B	0.031351	0.547073	1.096976	0.113*	0.5

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Nb1	0.02715 (17)	0.03660 (18)	0.02138 (16)	0.01177 (13)	0.00716 (12)	0.00606 (12)
N1	0.0242 (15)	0.0362 (15)	0.0222 (15)	0.0084 (13)	0.0040 (12)	0.0043 (12)
N2	0.0245 (14)	0.0384 (15)	0.0249 (15)	0.0103 (13)	0.0093 (12)	0.0081 (12)
N3	0.0491 (19)	0.0476 (19)	0.0368 (18)	0.0191 (16)	0.0159 (15)	0.0037 (15)
N4	0.0361 (18)	0.060 (2)	0.0347 (18)	0.0146 (16)	0.0127 (15)	0.0195 (16)
N5	0.064 (2)	0.057 (2)	0.049 (2)	0.0371 (19)	0.0206 (17)	0.0187 (16)
N6	0.0362 (19)	0.0517 (19)	0.0357 (18)	0.0103 (16)	−0.0012 (15)	0.0102 (15)
C1	0.0258 (17)	0.0289 (17)	0.0223 (17)	0.0113 (14)	0.0087 (14)	0.0056 (13)
C2	0.0263 (17)	0.0308 (17)	0.0250 (18)	0.0132 (15)	0.0079 (14)	0.0058 (14)
C3	0.0312 (19)	0.041 (2)	0.030 (2)	0.0126 (17)	0.0054 (16)	0.0093 (16)
C4	0.037 (2)	0.043 (2)	0.0255 (19)	0.0195 (18)	0.0058 (16)	0.0082 (16)
C5	0.039 (2)	0.044 (2)	0.031 (2)	0.0163 (18)	0.0136 (16)	0.0043 (16)
C6	0.043 (2)	0.043 (2)	0.0292 (19)	0.0215 (19)	0.0151 (17)	0.0114 (16)
C7	0.0286 (19)	0.049 (2)	0.0218 (18)	0.0041 (17)	0.0006 (15)	0.0120 (16)
C8	0.059 (3)	0.048 (2)	0.034 (2)	−0.002 (2)	−0.001 (2)	0.0081 (19)
C9	0.071 (4)	0.066 (3)	0.057 (3)	−0.024 (3)	−0.009 (3)	0.010 (2)
C10	0.042 (3)	0.140 (6)	0.076 (4)	−0.012 (4)	0.005 (3)	0.034 (4)
C11	0.032 (3)	0.140 (5)	0.062 (3)	0.024 (3)	0.013 (2)	0.033 (3)
C12	0.029 (2)	0.090 (3)	0.037 (2)	0.022 (2)	0.0102 (17)	0.022 (2)
C13	0.120 (4)	0.042 (2)	0.055 (3)	0.021 (3)	0.009 (3)	0.003 (2)
C14	0.064 (3)	0.103 (4)	0.056 (3)	0.055 (3)	0.023 (2)	0.013 (3)
C15	0.0268 (19)	0.054 (2)	0.0220 (18)	0.0073 (17)	0.0074 (15)	0.0128 (16)
C16	0.046 (2)	0.055 (3)	0.034 (2)	0.003 (2)	0.0076 (18)	0.0136 (19)
C17	0.064 (3)	0.069 (3)	0.052 (3)	−0.014 (3)	0.005 (2)	0.013 (2)
C18	0.040 (3)	0.136 (5)	0.066 (4)	−0.008 (3)	0.017 (3)	0.024 (4)
C19	0.036 (3)	0.142 (5)	0.055 (3)	0.026 (3)	0.018 (2)	0.024 (3)
C20	0.033 (2)	0.094 (3)	0.034 (2)	0.028 (2)	0.0151 (17)	0.022 (2)
C21	0.085 (3)	0.042 (2)	0.058 (3)	0.019 (2)	0.010 (2)	0.005 (2)
C22	0.060 (3)	0.108 (4)	0.056 (3)	0.058 (3)	0.026 (2)	0.015 (3)
C23	0.0287 (18)	0.0378 (19)	0.032 (2)	0.0108 (16)	0.0115 (15)	−0.0009 (16)
C24	0.032 (2)	0.044 (2)	0.040 (2)	0.0156 (17)	0.0099 (16)	0.0070 (17)
C25	0.046 (2)	0.043 (2)	0.050 (2)	0.0246 (19)	0.0153 (19)	0.0029 (18)
C26	0.049 (2)	0.046 (2)	0.038 (2)	0.0174 (19)	0.0146 (18)	−0.0019 (17)
C27	0.040 (2)	0.048 (2)	0.034 (2)	0.0174 (18)	0.0100 (17)	0.0080 (17)
C28	0.0305 (19)	0.041 (2)	0.040 (2)	0.0155 (16)	0.0116 (16)	0.0038 (17)
C29	0.067 (3)	0.059 (3)	0.049 (3)	0.031 (2)	0.010 (2)	0.013 (2)
C30	0.064 (3)	0.050 (2)	0.056 (3)	0.034 (2)	0.015 (2)	0.0103 (19)
C31	0.033 (2)	0.054 (2)	0.034 (2)	0.0147 (18)	0.0105 (16)	0.0217 (18)
C32	0.041 (2)	0.055 (2)	0.037 (2)	0.0157 (19)	0.0067 (18)	0.0144 (18)
C33	0.053 (3)	0.052 (2)	0.059 (3)	0.012 (2)	0.011 (2)	0.024 (2)
C34	0.049 (3)	0.080 (3)	0.080 (3)	0.019 (2)	0.035 (2)	0.044 (3)
C35	0.048 (3)	0.082 (3)	0.074 (3)	0.033 (2)	0.037 (2)	0.038 (3)
C36	0.037 (2)	0.061 (3)	0.052 (2)	0.023 (2)	0.0176 (19)	0.027 (2)
C37	0.082 (3)	0.066 (3)	0.055 (3)	0.026 (3)	0.020 (2)	0.004 (2)
C38	0.062 (3)	0.068 (3)	0.095 (4)	0.038 (2)	0.040 (3)	0.034 (3)
C39	0.032 (2)	0.0359 (19)	0.043 (2)	0.0132 (17)	0.0082 (17)	0.0081 (16)
C40	0.040 (2)	0.044 (2)	0.051 (2)	0.0190 (19)	0.0148 (19)	0.0062 (18)
C41	0.063 (3)	0.062 (3)	0.080 (3)	0.042 (2)	0.016 (3)	0.008 (2)
C42	0.083 (3)	0.066 (3)	0.076 (3)	0.046 (3)	0.011 (3)	0.028 (3)
C43	0.067 (3)	0.063 (3)	0.053 (3)	0.030 (2)	0.017 (2)	0.023 (2)
C44	0.036 (2)	0.043 (2)	0.040 (2)	0.0161 (17)	0.0085 (17)	0.0089 (17)
C45	0.086 (4)	0.083 (3)	0.075 (3)	0.045 (3)	0.040 (3)	0.010 (3)
C46	0.069 (3)	0.078 (3)	0.045 (2)	0.044 (3)	0.023 (2)	0.012 (2)
C47	0.030 (2)	0.048 (2)	0.037 (2)	0.0082 (18)	0.0029 (17)	0.0163 (18)
C48	0.047 (2)	0.064 (3)	0.042 (2)	0.024 (2)	0.0072 (19)	0.017 (2)
C49	0.036 (2)	0.073 (3)	0.071 (3)	0.021 (2)	0.010 (2)	0.029 (3)
C50	0.033 (2)	0.061 (3)	0.077 (3)	0.003 (2)	−0.008 (2)	0.030 (3)
C51	0.048 (3)	0.046 (2)	0.056 (3)	0.004 (2)	0.000 (2)	0.016 (2)
C52	0.031 (2)	0.044 (2)	0.045 (2)	0.0063 (18)	0.0050 (18)	0.0152 (18)
C53	0.080 (3)	0.112 (4)	0.054 (3)	0.058 (3)	0.013 (3)	0.007 (3)
C54	0.059 (3)	0.054 (3)	0.073 (3)	0.011 (2)	0.017 (2)	0.005 (2)
O1	0.116 (7)	0.180 (11)	0.213 (13)	0.089 (7)	0.060 (8)	0.038 (8)
C55	0.106 (7)	0.208 (9)	0.150 (8)	0.091 (7)	−0.003 (6)	−0.086 (7)
C56	0.111 (9)	0.147 (11)	0.182 (14)	0.037 (9)	0.033 (12)	0.011 (11)
C57	0.100 (9)	0.197 (11)	0.173 (17)	0.064 (9)	0.046 (10)	0.103 (12)
C58	0.106 (9)	0.179 (15)	0.086 (7)	0.091 (9)	0.025 (7)	0.020 (9)
O1'	0.117 (7)	0.243 (12)	0.191 (12)	0.063 (8)	0.054 (8)	0.019 (8)
C55'	0.106 (7)	0.208 (9)	0.150 (8)	0.091 (7)	−0.003 (6)	−0.086 (7)
C56'	0.087 (8)	0.140 (9)	0.122 (11)	0.043 (7)	0.044 (9)	0.004 (9)
C57'	0.121 (9)	0.220 (11)	0.155 (15)	0.031 (9)	0.065 (10)	0.104 (11)
C58'	0.125 (10)	0.231 (17)	0.080 (7)	0.052 (10)	0.031 (7)	0.024 (10)
O2	0.121 (7)	0.115 (6)	0.073 (5)	0.063 (6)	0.033 (5)	0.039 (4)
C59	0.076 (13)	0.102 (5)	0.14 (2)	0.050 (8)	0.047 (12)	0.080 (12)
C60	0.085 (12)	0.130 (16)	0.085 (6)	0.045 (13)	0.040 (5)	0.062 (5)
C61	0.076 (13)	0.102 (5)	0.14 (2)	0.050 (8)	0.047 (12)	0.080 (12)
C62	0.085 (12)	0.130 (16)	0.085 (6)	0.045 (13)	0.040 (5)	0.062 (5)

Geometric parameters (Å, º) top

Nb1—C3	2.045 (4)	C36—C38	1.501 (5)
Nb1—C5	2.061 (4)	C37—H37A	0.9800
Nb1—C6	2.109 (4)	C37—H37B	0.9800
Nb1—C4	2.112 (4)	C37—H37C	0.9800
Nb1—N1	2.259 (2)	C38—H38A	0.9800
Nb1—N2	2.261 (2)	C38—H38B	0.9800
N1—C1	1.319 (4)	C38—H38C	0.9800
N1—C7	1.441 (4)	C39—C44	1.389 (5)
N2—C2	1.312 (4)	C39—C40	1.402 (5)
N2—C15	1.436 (4)	C40—C41	1.380 (5)
N3—C3	1.196 (4)	C40—C45	1.502 (5)
N3—C23	1.388 (4)	C41—C42	1.378 (6)
N4—C4	1.174 (4)	C41—H41	0.9500
N4—C31	1.399 (4)	C42—C43	1.369 (6)
N5—C5	1.193 (4)	C42—H42	0.9500
N5—C39	1.383 (4)	C43—C44	1.378 (5)
N6—C6	1.175 (4)	C43—H43	0.9500
N6—C47	1.382 (4)	C44—C46	1.507 (5)
C1—C2	1.446 (4)	C45—H45A	0.9800
C1—C2ⁱ	1.458 (4)	C45—H45B	0.9800
C7—C8	1.396 (5)	C45—H45C	0.9800
C7—C12	1.396 (5)	C46—H46A	0.9800
C8—C9	1.405 (6)	C46—H46B	0.9800
C8—C13	1.494 (6)	C46—H46C	0.9800
C9—C10	1.352 (8)	C47—C52	1.389 (5)
C9—H9	0.9500	C47—C48	1.398 (5)
C10—C11	1.361 (8)	C48—C49	1.377 (5)
C10—H10	0.9500	C48—C53	1.501 (5)
C11—C12	1.402 (6)	C49—C50	1.365 (6)
C11—H11	0.9500	C49—H49	0.9500
C12—C14	1.486 (6)	C50—C51	1.377 (6)
C13—H13A	0.9800	C50—H50	0.9500
C13—H13B	0.9800	C51—C52	1.387 (5)
C13—H13C	0.9800	C51—H51	0.9500
C14—H14A	0.9800	C52—C54	1.504 (5)
C14—H14B	0.9800	C53—H53A	0.9800
C14—H14C	0.9800	C53—H53B	0.9800
C15—C16	1.396 (5)	C53—H53C	0.9800
C15—C20	1.403 (5)	C54—H54A	0.9800
C16—C17	1.403 (6)	C54—H54B	0.9800
C16—C21	1.489 (6)	C54—H54C	0.9800
C17—C18	1.379 (7)	O1—C58	1.439 (8)
C17—H17	0.9500	O1—C55	1.489 (8)
C18—C19	1.352 (7)	C55—C56	1.539 (8)
C18—H18	0.9500	C55—H55A	0.9900
C19—C20	1.395 (6)	C55—H55B	0.9900
C19—H19	0.9500	C56—C57	1.449 (9)
C20—C22	1.494 (6)	C56—H56A	0.9900
C21—H21A	0.9800	C56—H56B	0.9900
C21—H21B	0.9800	C57—C58	1.510 (8)
C21—H21C	0.9800	C57—H57A	0.9900
C22—H22A	0.9800	C57—H57B	0.9900
C22—H22B	0.9800	C58—H58A	0.9900
C22—H22C	0.9800	C58—H58B	0.9900
C23—C28	1.400 (4)	O1'—C58'	1.439 (8)
C23—C24	1.403 (4)	O1'—C55'	1.489 (8)
C24—C25	1.378 (5)	C55'—C56'	1.539 (8)
C24—C29	1.504 (5)	C55'—H55C	0.9900
C25—C26	1.378 (5)	C55'—H55D	0.9900
C25—H25	0.9500	C56'—C57'	1.450 (9)
C26—C27	1.383 (5)	C56'—H56C	0.9900
C26—H26	0.9500	C56'—H56D	0.9900
C27—C28	1.376 (4)	C57'—C58'	1.510 (8)
C27—H27	0.9500	C57'—H57C	0.9900
C28—C30	1.505 (4)	C57'—H57D	0.9900
C29—H29A	0.9800	C58'—H58C	0.9900
C29—H29B	0.9800	C58'—H58D	0.9900
C29—H29C	0.9800	O2—C59	1.35 (2)
C30—H30A	0.9800	O2—C62	1.37 (2)
C30—H30B	0.9800	C59—C60	1.488 (12)
C30—H30C	0.9800	C59—H59A	0.9900
C31—C32	1.393 (5)	C59—H59B	0.9900
C31—C36	1.400 (5)	C60—C61	1.505 (15)
C32—C33	1.377 (5)	C60—H60A	0.9900
C32—C37	1.506 (5)	C60—H60B	0.9900
C33—C34	1.375 (6)	C61—C62	1.491 (12)
C33—H33	0.9500	C61—H61A	0.9900
C34—C35	1.375 (6)	C61—H61B	0.9900
C34—H34	0.9500	C62—H62A	0.9900
C35—C36	1.388 (5)	C62—H62B	0.9900
C35—H35	0.9500

C3—Nb1—C5	111.28 (12)	H37A—C37—H37B	109.5
C3—Nb1—C6	71.98 (12)	C32—C37—H37C	109.5
C5—Nb1—C6	72.25 (13)	H37A—C37—H37C	109.5
C3—Nb1—C4	71.43 (13)	H37B—C37—H37C	109.5
C5—Nb1—C4	73.17 (13)	C36—C38—H38A	109.5
C6—Nb1—C4	114.44 (12)	C36—C38—H38B	109.5
C3—Nb1—N1	119.74 (11)	H38A—C38—H38B	109.5
C5—Nb1—N1	112.71 (11)	C36—C38—H38C	109.5
C6—Nb1—N1	84.55 (11)	H38A—C38—H38C	109.5
C4—Nb1—N1	160.83 (10)	H38B—C38—H38C	109.5
C3—Nb1—N2	114.55 (11)	N5—C39—C44	119.4 (3)
C5—Nb1—N2	117.44 (11)	N5—C39—C40	118.5 (3)
C6—Nb1—N2	161.93 (10)	C44—C39—C40	122.0 (3)
C4—Nb1—N2	83.52 (11)	C41—C40—C39	117.5 (4)
N1—Nb1—N2	77.62 (9)	C41—C40—C45	121.7 (4)
C1—N1—C7	119.5 (3)	C39—C40—C45	120.8 (3)
C1—N1—Nb1	108.92 (19)	C42—C41—C40	121.1 (4)
C7—N1—Nb1	131.08 (19)	C42—C41—H41	119.4
C2—N2—C15	122.5 (3)	C40—C41—H41	119.4
C2—N2—Nb1	109.19 (19)	C43—C42—C41	120.1 (4)
C15—N2—Nb1	127.79 (19)	C43—C42—H42	119.9
C3—N3—C23	163.7 (3)	C41—C42—H42	119.9
C4—N4—C31	178.3 (4)	C42—C43—C44	121.2 (4)
C5—N5—C39	165.0 (3)	C42—C43—H43	119.4
C6—N6—C47	168.6 (4)	C44—C43—H43	119.4
N1—C1—C2	121.9 (3)	C43—C44—C39	118.0 (3)
N1—C1—C2ⁱ	147.8 (3)	C43—C44—C46	121.3 (3)
C2—C1—C2ⁱ	90.3 (2)	C39—C44—C46	120.7 (3)
N2—C2—C1	121.7 (3)	C40—C45—H45A	109.5
N2—C2—C1ⁱ	148.6 (3)	C40—C45—H45B	109.5
C1—C2—C1ⁱ	89.7 (2)	H45A—C45—H45B	109.5
N3—C3—Nb1	178.6 (3)	C40—C45—H45C	109.5
N4—C4—Nb1	178.3 (3)	H45A—C45—H45C	109.5
N5—C5—Nb1	178.4 (3)	H45B—C45—H45C	109.5
N6—C6—Nb1	176.8 (3)	C44—C46—H46A	109.5
C8—C7—C12	121.6 (4)	C44—C46—H46B	109.5
C8—C7—N1	118.6 (3)	H46A—C46—H46B	109.5
C12—C7—N1	119.8 (3)	C44—C46—H46C	109.5
C7—C8—C9	117.7 (5)	H46A—C46—H46C	109.5
C7—C8—C13	121.7 (4)	H46B—C46—H46C	109.5
C9—C8—C13	120.6 (4)	N6—C47—C52	118.5 (3)
C10—C9—C8	120.6 (5)	N6—C47—C48	118.9 (3)
C10—C9—H9	119.7	C52—C47—C48	122.5 (3)
C8—C9—H9	119.7	C49—C48—C47	117.5 (4)
C9—C10—C11	121.7 (5)	C49—C48—C53	122.7 (4)
C9—C10—H10	119.2	C47—C48—C53	119.8 (4)
C11—C10—H10	119.2	C50—C49—C48	121.2 (4)
C10—C11—C12	120.4 (5)	C50—C49—H49	119.4
C10—C11—H11	119.8	C48—C49—H49	119.4
C12—C11—H11	119.8	C49—C50—C51	120.8 (4)
C7—C12—C11	117.9 (4)	C49—C50—H50	119.6
C7—C12—C14	120.8 (3)	C51—C50—H50	119.6
C11—C12—C14	121.2 (4)	C50—C51—C52	120.6 (4)
C8—C13—H13A	109.5	C50—C51—H51	119.7
C8—C13—H13B	109.5	C52—C51—H51	119.7
H13A—C13—H13B	109.5	C51—C52—C47	117.5 (4)
C8—C13—H13C	109.5	C51—C52—C54	122.0 (4)
H13A—C13—H13C	109.5	C47—C52—C54	120.5 (3)
H13B—C13—H13C	109.5	C48—C53—H53A	109.5
C12—C14—H14A	109.5	C48—C53—H53B	109.5
C12—C14—H14B	109.5	H53A—C53—H53B	109.5
H14A—C14—H14B	109.5	C48—C53—H53C	109.5
C12—C14—H14C	109.5	H53A—C53—H53C	109.5
H14A—C14—H14C	109.5	H53B—C53—H53C	109.5
H14B—C14—H14C	109.5	C52—C54—H54A	109.5
C16—C15—C20	121.9 (3)	C52—C54—H54B	109.5
C16—C15—N2	119.2 (3)	H54A—C54—H54B	109.5
C20—C15—N2	118.6 (3)	C52—C54—H54C	109.5
C15—C16—C17	118.0 (4)	H54A—C54—H54C	109.5
C15—C16—C21	120.9 (3)	H54B—C54—H54C	109.5
C17—C16—C21	121.1 (4)	C58—O1—C55	106.2 (6)
C18—C17—C16	120.2 (5)	O1—C55—C56	100.9 (7)
C18—C17—H17	119.9	O1—C55—H55A	111.6
C16—C17—H17	119.9	C56—C55—H55A	111.6
C19—C18—C17	120.9 (5)	O1—C55—H55B	111.6
C19—C18—H18	119.6	C56—C55—H55B	111.6
C17—C18—H18	119.6	H55A—C55—H55B	109.4
C18—C19—C20	121.9 (5)	C57—C56—C55	96.1 (7)
C18—C19—H19	119.1	C57—C56—H56A	112.5
C20—C19—H19	119.1	C55—C56—H56A	112.5
C19—C20—C15	117.2 (4)	C57—C56—H56B	112.5
C19—C20—C22	121.1 (4)	C55—C56—H56B	112.5
C15—C20—C22	121.7 (3)	H56A—C56—H56B	110.0
C16—C21—H21A	109.5	C56—C57—C58	99.7 (8)
C16—C21—H21B	109.5	C56—C57—H57A	111.8
H21A—C21—H21B	109.5	C58—C57—H57A	111.8
C16—C21—H21C	109.5	C56—C57—H57B	111.8
H21A—C21—H21C	109.5	C58—C57—H57B	111.8
H21B—C21—H21C	109.5	H57A—C57—H57B	109.5
C20—C22—H22A	109.5	O1—C58—C57	103.5 (7)
C20—C22—H22B	109.5	O1—C58—H58A	111.1
H22A—C22—H22B	109.5	C57—C58—H58A	111.1
C20—C22—H22C	109.5	O1—C58—H58B	111.1
H22A—C22—H22C	109.5	C57—C58—H58B	111.1
H22B—C22—H22C	109.5	H58A—C58—H58B	109.0
N3—C23—C28	119.5 (3)	C58'—O1'—C55'	106.3 (6)
N3—C23—C24	118.1 (3)	O1'—C55'—C56'	101.2 (7)
C28—C23—C24	122.4 (3)	O1'—C55'—H55C	111.5
C25—C24—C23	117.2 (3)	C56'—C55'—H55C	111.5
C25—C24—C29	122.6 (3)	O1'—C55'—H55D	111.5
C23—C24—C29	120.3 (3)	C56'—C55'—H55D	111.5
C26—C25—C24	121.8 (3)	H55C—C55'—H55D	109.4
C26—C25—H25	119.1	C57'—C56'—C55'	96.2 (7)
C24—C25—H25	119.1	C57'—C56'—H56C	112.5
C25—C26—C27	119.7 (3)	C55'—C56'—H56C	112.5
C25—C26—H26	120.2	C57'—C56'—H56D	112.5
C27—C26—H26	120.2	C55'—C56'—H56D	112.5
C28—C27—C26	121.4 (3)	H56C—C56'—H56D	110.0
C28—C27—H27	119.3	C56'—C57'—C58'	99.4 (8)
C26—C27—H27	119.3	C56'—C57'—H57C	111.9
C27—C28—C23	117.6 (3)	C58'—C57'—H57C	111.9
C27—C28—C30	121.8 (3)	C56'—C57'—H57D	111.9
C23—C28—C30	120.6 (3)	C58'—C57'—H57D	111.9
C24—C29—H29A	109.5	H57C—C57'—H57D	109.6
C24—C29—H29B	109.5	O1'—C58'—C57'	103.2 (7)
H29A—C29—H29B	109.5	O1'—C58'—H58C	111.1
C24—C29—H29C	109.5	C57'—C58'—H58C	111.1
H29A—C29—H29C	109.5	O1'—C58'—H58D	111.1
H29B—C29—H29C	109.5	C57'—C58'—H58D	111.1
C28—C30—H30A	109.5	H58C—C58'—H58D	109.1
C28—C30—H30B	109.5	C59—O2—C62	111 (2)
H30A—C30—H30B	109.5	O2—C59—C60	105.8 (18)
C28—C30—H30C	109.5	O2—C59—H59A	110.6
H30A—C30—H30C	109.5	C60—C59—H59A	110.6
H30B—C30—H30C	109.5	O2—C59—H59B	110.6
C32—C31—N4	118.2 (3)	C60—C59—H59B	110.6
C32—C31—C36	123.5 (3)	H59A—C59—H59B	108.7
N4—C31—C36	118.3 (3)	C59—C60—C61	105.2 (10)
C33—C32—C31	117.1 (4)	C59—C60—H60A	110.7
C33—C32—C37	122.0 (4)	C61—C60—H60A	110.7
C31—C32—C37	120.8 (3)	C59—C60—H60B	110.7
C34—C33—C32	121.2 (4)	C61—C60—H60B	110.7
C34—C33—H33	119.4	H60A—C60—H60B	108.8
C32—C33—H33	119.4	C62—C61—C60	103.6 (9)
C33—C34—C35	120.5 (4)	C62—C61—H61A	111.0
C33—C34—H34	119.8	C60—C61—H61A	111.0
C35—C34—H34	119.8	C62—C61—H61B	111.0
C34—C35—C36	121.3 (4)	C60—C61—H61B	111.0
C34—C35—H35	119.3	H61A—C61—H61B	109.0
C36—C35—H35	119.3	O2—C62—C61	105.7 (17)
C35—C36—C31	116.3 (4)	O2—C62—H62A	110.6
C35—C36—C38	121.7 (4)	C61—C62—H62A	110.6
C31—C36—C38	121.9 (3)	O2—C62—H62B	110.6
C32—C37—H37A	109.5	C61—C62—H62B	110.6
C32—C37—H37B	109.5	H62A—C62—H62B	108.7

C7—N1—C1—C2	179.4 (3)	C24—C23—C28—C30	−179.7 (3)
Nb1—N1—C1—C2	6.3 (3)	N4—C31—C32—C33	178.3 (3)
C7—N1—C1—C2ⁱ	−1.4 (6)	C36—C31—C32—C33	−1.2 (5)
Nb1—N1—C1—C2ⁱ	−174.5 (4)	N4—C31—C32—C37	−2.1 (5)
C15—N2—C2—C1	−177.9 (3)	C36—C31—C32—C37	178.5 (3)
Nb1—N2—C2—C1	−5.7 (3)	C31—C32—C33—C34	0.5 (6)
C15—N2—C2—C1ⁱ	2.1 (7)	C37—C32—C33—C34	−179.2 (4)
Nb1—N2—C2—C1ⁱ	174.2 (4)	C32—C33—C34—C35	0.1 (6)
N1—C1—C2—N2	−0.5 (4)	C33—C34—C35—C36	−0.1 (7)
C2ⁱ—C1—C2—N2	180.0 (4)	C34—C35—C36—C31	−0.5 (6)
N1—C1—C2—C1ⁱ	179.6 (3)	C34—C35—C36—C38	179.9 (4)
C2ⁱ—C1—C2—C1ⁱ	0.004 (1)	C32—C31—C36—C35	1.2 (5)
C1—N1—C7—C8	110.8 (3)	N4—C31—C36—C35	−178.3 (3)
Nb1—N1—C7—C8	−77.9 (4)	C32—C31—C36—C38	−179.2 (3)
C1—N1—C7—C12	−71.3 (4)	N4—C31—C36—C38	1.3 (5)
Nb1—N1—C7—C12	99.9 (3)	C5—N5—C39—C44	8.1 (16)
C12—C7—C8—C9	1.1 (5)	C5—N5—C39—C40	−170.7 (13)
N1—C7—C8—C9	179.0 (3)	N5—C39—C40—C41	179.9 (3)
C12—C7—C8—C13	−177.9 (3)	C44—C39—C40—C41	1.1 (5)
N1—C7—C8—C13	−0.1 (5)	N5—C39—C40—C45	1.0 (5)
C7—C8—C9—C10	0.8 (7)	C44—C39—C40—C45	−177.7 (4)
C13—C8—C9—C10	179.8 (5)	C39—C40—C41—C42	−0.7 (6)
C8—C9—C10—C11	−1.5 (8)	C45—C40—C41—C42	178.1 (4)
C9—C10—C11—C12	0.2 (8)	C40—C41—C42—C43	−0.3 (7)
C8—C7—C12—C11	−2.3 (5)	C41—C42—C43—C44	1.1 (7)
N1—C7—C12—C11	179.9 (3)	C42—C43—C44—C39	−0.7 (6)
C8—C7—C12—C14	174.9 (3)	C42—C43—C44—C46	−179.7 (4)
N1—C7—C12—C14	−3.0 (5)	N5—C39—C44—C43	−179.2 (3)
C10—C11—C12—C7	1.7 (6)	C40—C39—C44—C43	−0.5 (5)
C10—C11—C12—C14	−175.5 (4)	N5—C39—C44—C46	−0.2 (5)
C2—N2—C15—C16	75.4 (4)	C40—C39—C44—C46	178.5 (3)
Nb1—N2—C15—C16	−95.2 (3)	C6—N6—C47—C52	171.4 (16)
C2—N2—C15—C20	−110.6 (4)	C6—N6—C47—C48	−9.8 (19)
Nb1—N2—C15—C20	78.8 (4)	N6—C47—C48—C49	−179.5 (3)
C20—C15—C16—C17	1.6 (5)	C52—C47—C48—C49	−0.7 (5)
N2—C15—C16—C17	175.4 (3)	N6—C47—C48—C53	−1.6 (5)
C20—C15—C16—C21	−176.9 (3)	C52—C47—C48—C53	177.2 (4)
N2—C15—C16—C21	−3.2 (5)	C47—C48—C49—C50	−0.2 (6)
C15—C16—C17—C18	−0.6 (6)	C53—C48—C49—C50	−178.1 (4)
C21—C16—C17—C18	178.0 (4)	C48—C49—C50—C51	0.8 (6)
C16—C17—C18—C19	0.0 (8)	C49—C50—C51—C52	−0.5 (6)
C17—C18—C19—C20	−0.4 (8)	C50—C51—C52—C47	−0.4 (5)
C18—C19—C20—C15	1.4 (6)	C50—C51—C52—C54	178.8 (4)
C18—C19—C20—C22	−177.8 (4)	N6—C47—C52—C51	179.8 (3)
C16—C15—C20—C19	−2.0 (5)	C48—C47—C52—C51	1.0 (5)
N2—C15—C20—C19	−175.8 (3)	N6—C47—C52—C54	0.6 (5)
C16—C15—C20—C22	177.2 (3)	C48—C47—C52—C54	−178.2 (3)
N2—C15—C20—C22	3.4 (5)	C58—O1—C55—C56	23.2 (14)
C3—N3—C23—C28	−17.5 (13)	O1—C55—C56—C57	−49.1 (13)
C3—N3—C23—C24	162.2 (11)	C55—C56—C57—C58	55.7 (14)
N3—C23—C24—C25	−178.5 (3)	C55—O1—C58—C57	10.8 (16)
C28—C23—C24—C25	1.2 (5)	C56—C57—C58—O1	−43.2 (15)
N3—C23—C24—C29	1.3 (5)	C58'—O1'—C55'—C56'	21.5 (14)
C28—C23—C24—C29	−179.0 (3)	O1'—C55'—C56'—C57'	−48.3 (13)
C23—C24—C25—C26	−1.3 (5)	C55'—C56'—C57'—C58'	56.1 (14)
C29—C24—C25—C26	178.9 (4)	C55'—O1'—C58'—C57'	12.8 (16)
C24—C25—C26—C27	0.7 (6)	C56'—C57'—C58'—O1'	−44.7 (15)
C25—C26—C27—C28	0.1 (5)	C62—O2—C59—C60	29 (3)
C26—C27—C28—C23	−0.2 (5)	O2—C59—C60—C61	−15 (4)
C26—C27—C28—C30	179.1 (3)	C59—C60—C61—C62	−2 (6)
N3—C23—C28—C27	179.2 (3)	C59—O2—C62—C61	−31 (4)
C24—C23—C28—C27	−0.5 (5)	C60—C61—C62—O2	19 (5)
N3—C23—C28—C30	−0.1 (5)

Symmetry code: (i) −x+1, −y+1, −z+1.

Hexakis(2,6-diisopropylphenyl isocyanide)niobium(0) (3) top

Crystal data top

[Nb(C₁₃H₁₇N)₆]	D_x = 1.124 Mg m⁻³
M_r = 1216.56	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3:H	Cell parameters from 2975 reflections
a = 15.2582 (10) Å	θ = 2.2–21.4°
c = 26.7313 (17) Å	µ = 0.21 mm⁻¹
V = 5389.6 (8) Å³	T = 173 K
Z = 3	Block, red
F(000) = 1959	0.20 × 0.20 × 0.20 mm

Data collection top

Bruker APEXII CCD platform diffractometer	2752 independent reflections
Radiation source: normal-focus sealed tube	2606 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.046
area detector, ω scans	θ_max = 27.5°, θ_min = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2012)	h = −19→19
T_min = 0.691, T_max = 0.746	k = −19→19
21272 measured reflections	l = −34→34

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)] = 0.035	Hydrogen site location: mixed
wR(F²) = 0.085	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0354P)² + 7.2006P] where P = (F_o² + 2F_c²)/3
2752 reflections	(Δ/σ)_max < 0.001
193 parameters	Δρ_max = 0.26 e Å⁻³
341 restraints	Δρ_min = −0.36 e Å⁻³

Special details top

Refinement. The Nb atom is on a crystallographic -3 position, and thus one-sixth of the molecule is unique. The isocyanide ligand is modeled as disordered over two positions, anchored at carbon atom C1 (0.547 (3):0.453 (3)). Analogous bond lengths and angles between the two positions were restrained to be similar. Anisotropic displacement parameters for proximal atoms were constrained to be equivalent. Additionally, anisotropic displacement parameters over the entire asymmetric unit were heavily restrained to be similar.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Nb1	0.000000	0.000000	0.000000	0.02289 (11)
C1	0.07125 (12)	0.13928 (12)	0.04187 (6)	0.0309 (3)	0.547 (3)
N1	0.1230 (4)	0.2219 (3)	0.0583 (2)	0.0326 (10)	0.547 (3)
C2	0.1871 (4)	0.31814 (19)	0.07710 (18)	0.0282 (11)	0.547 (3)
C3	0.2023 (3)	0.4013 (3)	0.04831 (12)	0.0327 (8)	0.547 (3)
C4	0.2706 (3)	0.4964 (3)	0.0667 (2)	0.0377 (11)	0.547 (3)
H4A	0.282894	0.554679	0.048242	0.045*	0.547 (3)
C5	0.3209 (7)	0.5084 (4)	0.1110 (3)	0.0410 (13)	0.547 (3)
H5A	0.368891	0.574376	0.122173	0.049*	0.547 (3)
C6	0.3024 (8)	0.4257 (5)	0.1391 (3)	0.0400 (5)	0.547 (3)
H6A	0.336129	0.435568	0.170258	0.048*	0.547 (3)
C7	0.2355 (6)	0.3280 (4)	0.1231 (2)	0.0338 (4)	0.547 (3)
C8	0.2141 (9)	0.2355 (7)	0.1536 (3)	0.0476 (7)	0.547 (3)
H8A	0.207461	0.182248	0.129546	0.057*	0.547 (3)
C9	0.1143 (16)	0.1934 (19)	0.1814 (12)	0.077 (2)	0.547 (3)
H9A	0.060535	0.182215	0.157833	0.115*	0.547 (3)
H9B	0.119972	0.241694	0.207151	0.115*	0.547 (3)
H9C	0.098070	0.129056	0.197256	0.115*	0.547 (3)
C10	0.2996 (17)	0.2557 (16)	0.1895 (12)	0.0835 (19)	0.547 (3)
H10A	0.364386	0.290804	0.171794	0.125*	0.547 (3)
H10B	0.289363	0.191306	0.202727	0.125*	0.547 (3)
H10C	0.299969	0.297948	0.217242	0.125*	0.547 (3)
C11	0.1481 (3)	0.3869 (3)	−0.00123 (13)	0.0481 (10)	0.547 (3)
H11A	0.143270	0.326138	−0.018029	0.058*	0.547 (3)
C12	0.0409 (3)	0.3659 (4)	0.00837 (17)	0.0732 (15)	0.547 (3)
H12A	0.005078	0.305903	0.029689	0.110*	0.547 (3)
H12B	0.004998	0.353874	−0.023538	0.110*	0.547 (3)
H12C	0.043520	0.424264	0.025142	0.110*	0.547 (3)
C13	0.2024 (4)	0.4762 (3)	−0.03649 (15)	0.0735 (14)	0.547 (3)
H13A	0.273258	0.493620	−0.039798	0.110*	0.547 (3)
H13B	0.199289	0.534343	−0.023075	0.110*	0.547 (3)
H13C	0.169688	0.458219	−0.069386	0.110*	0.547 (3)
C1'	0.07125 (12)	0.13928 (12)	0.04187 (6)	0.0309 (3)	0.453 (3)
N1'	0.1008 (6)	0.2137 (3)	0.0665 (3)	0.0326 (10)	0.453 (3)
C2'	0.1663 (6)	0.3122 (2)	0.0824 (2)	0.0282 (11)	0.453 (3)
C3'	0.1688 (3)	0.3924 (3)	0.05563 (15)	0.0327 (8)	0.453 (3)
C4'	0.2395 (4)	0.4894 (3)	0.0708 (3)	0.0377 (11)	0.453 (3)
H4B	0.244304	0.545772	0.053187	0.045*	0.453 (3)
C5'	0.3025 (9)	0.5060 (5)	0.1107 (4)	0.0410 (13)	0.453 (3)
H5B	0.349890	0.573267	0.120430	0.049*	0.453 (3)
C6'	0.2978 (10)	0.4261 (6)	0.1366 (4)	0.0400 (5)	0.453 (3)
H6B	0.341772	0.438921	0.164207	0.048*	0.453 (3)
C7'	0.2300 (7)	0.3269 (5)	0.1232 (2)	0.0338 (4)	0.453 (3)
C8'	0.2209 (11)	0.2366 (8)	0.1517 (4)	0.0476 (7)	0.453 (3)
H8B	0.219543	0.187515	0.126478	0.057*	0.453 (3)
C9'	0.1219 (19)	0.184 (2)	0.1806 (15)	0.077 (2)	0.453 (3)
H9D	0.063325	0.158504	0.157916	0.115*	0.453 (3)
H9E	0.122258	0.235233	0.202910	0.115*	0.453 (3)
H9F	0.116611	0.126501	0.200274	0.115*	0.453 (3)
C10'	0.310 (2)	0.265 (2)	0.1863 (15)	0.0835 (19)	0.453 (3)
H10D	0.374915	0.300197	0.167868	0.125*	0.453 (3)
H10E	0.303073	0.202279	0.201305	0.125*	0.453 (3)
H10F	0.310046	0.309804	0.212562	0.125*	0.453 (3)
C11'	0.0987 (4)	0.3722 (3)	0.01170 (14)	0.0406 (11)	0.453 (3)
H11B	0.037378	0.304934	0.018218	0.049*	0.453 (3)
C12'	0.0616 (5)	0.4477 (5)	0.0080 (2)	0.0687 (16)	0.453 (3)
H12D	0.006092	0.423188	−0.016282	0.103*	0.453 (3)
H12E	0.117266	0.513325	−0.003055	0.103*	0.453 (3)
H12F	0.037522	0.455198	0.040781	0.103*	0.453 (3)
C13'	0.1426 (4)	0.3616 (5)	−0.03709 (15)	0.0678 (16)	0.453 (3)
H13D	0.095819	0.351707	−0.064475	0.102*	0.453 (3)
H13E	0.152718	0.303075	−0.035197	0.102*	0.453 (3)
H13F	0.207670	0.422946	−0.043247	0.102*	0.453 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Nb1	0.02093 (12)	0.02093 (12)	0.02681 (18)	0.01047 (6)	0.000	0.000
C1	0.0336 (8)	0.0277 (8)	0.0338 (8)	0.0170 (7)	−0.0032 (6)	−0.0023 (6)
N1	0.031 (3)	0.0278 (9)	0.0328 (19)	0.0103 (10)	0.0069 (16)	−0.0040 (11)
C2	0.024 (3)	0.0248 (8)	0.0320 (12)	0.0097 (9)	0.0080 (16)	−0.0062 (8)
C3	0.033 (2)	0.0317 (11)	0.0335 (13)	0.0161 (15)	0.0035 (14)	−0.0037 (9)
C4	0.040 (3)	0.0268 (10)	0.0432 (13)	0.0144 (15)	0.006 (2)	0.0009 (9)
C5	0.034 (3)	0.0284 (9)	0.0517 (11)	0.0089 (12)	−0.0019 (15)	−0.0111 (8)
C6	0.0393 (12)	0.0401 (9)	0.0392 (11)	0.0189 (8)	−0.0069 (8)	−0.0115 (8)
C7	0.0362 (10)	0.0320 (8)	0.0338 (8)	0.0175 (7)	0.0024 (7)	−0.0049 (6)
C8	0.0591 (17)	0.0398 (10)	0.0444 (12)	0.0251 (11)	−0.0030 (11)	0.0007 (8)
C9	0.087 (3)	0.066 (4)	0.0761 (19)	0.0375 (19)	0.029 (2)	0.029 (3)
C10	0.105 (4)	0.072 (3)	0.080 (3)	0.049 (3)	−0.031 (4)	0.003 (2)
C11	0.058 (3)	0.045 (2)	0.045 (2)	0.028 (2)	−0.0046 (19)	−0.0044 (17)
C12	0.063 (3)	0.092 (4)	0.062 (3)	0.037 (3)	−0.022 (2)	−0.011 (3)
C13	0.091 (4)	0.082 (3)	0.044 (2)	0.041 (3)	−0.004 (2)	0.014 (2)
C1'	0.0336 (8)	0.0277 (8)	0.0338 (8)	0.0170 (7)	−0.0032 (6)	−0.0023 (6)
N1'	0.031 (3)	0.0278 (9)	0.0328 (19)	0.0103 (10)	0.0069 (16)	−0.0040 (11)
C2'	0.024 (3)	0.0248 (8)	0.0320 (12)	0.0097 (9)	0.0080 (16)	−0.0062 (8)
C3'	0.033 (2)	0.0317 (11)	0.0335 (13)	0.0161 (15)	0.0035 (14)	−0.0037 (9)
C4'	0.040 (3)	0.0268 (10)	0.0432 (13)	0.0144 (15)	0.006 (2)	0.0009 (9)
C5'	0.034 (3)	0.0284 (9)	0.0517 (11)	0.0089 (12)	−0.0019 (15)	−0.0111 (8)
C6'	0.0393 (12)	0.0401 (9)	0.0392 (11)	0.0189 (8)	−0.0069 (8)	−0.0115 (8)
C7'	0.0362 (10)	0.0320 (8)	0.0338 (8)	0.0175 (7)	0.0024 (7)	−0.0049 (6)
C8'	0.0591 (17)	0.0398 (10)	0.0444 (12)	0.0251 (11)	−0.0030 (11)	0.0007 (8)
C9'	0.087 (3)	0.066 (4)	0.0761 (19)	0.0375 (19)	0.029 (2)	0.029 (3)
C10'	0.105 (4)	0.072 (3)	0.080 (3)	0.049 (3)	−0.031 (4)	0.003 (2)
C11'	0.044 (3)	0.040 (2)	0.038 (2)	0.022 (3)	−0.004 (2)	0.0000 (18)
C12'	0.086 (4)	0.073 (4)	0.066 (3)	0.054 (3)	−0.022 (3)	−0.006 (3)
C13'	0.070 (3)	0.090 (4)	0.034 (2)	0.033 (3)	−0.006 (2)	−0.012 (3)

Geometric parameters (Å, º) top

Nb1—C1ⁱ	2.1542 (15)	C13—H13A	0.9800
Nb1—C1ⁱⁱ	2.1541 (15)	C13—H13B	0.9800
Nb1—C1ⁱⁱⁱ	2.1541 (15)	C13—H13C	0.9800
Nb1—C1'	2.1542 (15)	C1'—N1'	1.189 (2)
Nb1—C1	2.1542 (15)	N1'—C2'	1.391 (2)
Nb1—C1^iv	2.1542 (15)	C2'—C3'	1.401 (3)
Nb1—C1^v	2.1542 (15)	C2'—C7'	1.403 (3)
C1—N1	1.187 (2)	C3'—C4'	1.387 (3)
N1—C2	1.389 (2)	C3'—C11'	1.513 (3)
C2—C3	1.401 (3)	C4'—C5'	1.372 (3)
C2—C7	1.404 (3)	C4'—H4B	0.9500
C3—C4	1.387 (3)	C5'—C6'	1.372 (3)
C3—C11	1.518 (3)	C5'—H5B	0.9500
C4—C5	1.371 (3)	C6'—C7'	1.386 (3)
C4—H4A	0.9500	C6'—H6B	0.9500
C5—C6	1.372 (3)	C7'—C8'	1.518 (3)
C5—H5A	0.9500	C8'—C9'	1.520 (4)
C6—C7	1.387 (3)	C8'—C10'	1.522 (4)
C6—H6A	0.9500	C8'—H8B	1.0000
C7—C8	1.518 (3)	C9'—H9D	0.9853
C8—C9	1.519 (4)	C9'—H9E	0.9855
C8—C10	1.523 (3)	C9'—H9F	0.9868
C8—H8A	1.0000	C10'—H10D	0.9874
C9—H9A	0.9800	C10'—H10E	0.9889
C9—H9B	0.9800	C10'—H10F	0.9831
C9—H9C	0.9800	C11'—C13'	1.512 (4)
C10—H10A	0.9800	C11'—C12'	1.519 (3)
C10—H10B	0.9800	C11'—H11B	1.0000
C10—H10C	0.9800	C12'—H12D	0.9800
C11—C13	1.517 (3)	C12'—H12E	0.9800
C11—C12	1.523 (3)	C12'—H12F	0.9800
C11—H11A	1.0000	C13'—H13D	0.9800
C12—H12A	0.9800	C13'—H13E	0.9800
C12—H12B	0.9800	C13'—H13F	0.9800
C12—H12C	0.9800

C1ⁱ—Nb1—C1ⁱⁱ	95.46 (6)	H12A—C12—H12C	109.5
C1ⁱ—Nb1—C1ⁱⁱⁱ	84.54 (6)	H12B—C12—H12C	109.5
C1ⁱⁱ—Nb1—C1ⁱⁱⁱ	180.00 (15)	C11—C13—H13A	109.5
C1ⁱ—Nb1—C1	180.0	C11—C13—H13B	109.5
C1ⁱⁱ—Nb1—C1	84.54 (6)	H13A—C13—H13B	109.5
C1ⁱⁱⁱ—Nb1—C1	95.46 (6)	C11—C13—H13C	109.5
C1ⁱ—Nb1—C1^iv	95.46 (6)	H13A—C13—H13C	109.5
C1ⁱⁱ—Nb1—C1^iv	95.46 (6)	H13B—C13—H13C	109.5
C1ⁱⁱⁱ—Nb1—C1^iv	84.54 (6)	N1'—C1'—Nb1	173.2 (4)
C1'—Nb1—C1^iv	84.54 (6)	C1'—N1'—C2'	157.7 (6)
C1—Nb1—C1^iv	84.54 (6)	N1'—C2'—C3'	118.7 (4)
C1ⁱ—Nb1—C1^v	84.54 (6)	N1'—C2'—C7'	118.4 (4)
C1ⁱⁱ—Nb1—C1^v	84.54 (6)	C3'—C2'—C7'	122.8 (3)
C1ⁱⁱⁱ—Nb1—C1^v	95.46 (6)	C4'—C3'—C2'	116.8 (3)
C1'—Nb1—C1^v	95.46 (6)	C4'—C3'—C11'	122.5 (4)
C1—Nb1—C1^v	95.46 (6)	C2'—C3'—C11'	120.7 (3)
C1^iv—Nb1—C1^v	180.00 (10)	C5'—C4'—C3'	121.5 (4)
N1—C1—Nb1	168.3 (3)	C5'—C4'—H4B	119.3
C1—N1—C2	177.6 (6)	C3'—C4'—H4B	119.3
N1—C2—C3	118.0 (3)	C6'—C5'—C4'	120.5 (4)
N1—C2—C7	119.0 (3)	C6'—C5'—H5B	119.7
C3—C2—C7	123.0 (3)	C4'—C5'—H5B	119.7
C4—C3—C2	116.8 (3)	C5'—C6'—C7'	121.2 (4)
C4—C3—C11	122.1 (3)	C5'—C6'—H6B	119.4
C2—C3—C11	121.1 (3)	C7'—C6'—H6B	119.4
C5—C4—C3	121.5 (3)	C6'—C7'—C2'	117.1 (3)
C5—C4—H4A	119.2	C6'—C7'—C8'	122.7 (4)
C3—C4—H4A	119.2	C2'—C7'—C8'	120.2 (4)
C6—C5—C4	120.5 (3)	C7'—C8'—C9'	110.7 (4)
C6—C5—H5A	119.8	C7'—C8'—C10'	112.7 (5)
C4—C5—H5A	119.8	C9'—C8'—C10'	110.6 (5)
C5—C6—C7	121.4 (3)	C7'—C8'—H8B	107.5
C5—C6—H6A	119.3	C9'—C8'—H8B	107.5
C7—C6—H6A	119.3	C10'—C8'—H8B	107.5
C6—C7—C2	116.8 (3)	C8'—C9'—H9D	111.2
C6—C7—C8	122.3 (3)	C8'—C9'—H9E	106.0
C2—C7—C8	120.9 (3)	H9D—C9'—H9E	109.0
C7—C8—C9	111.1 (4)	C8'—C9'—H9F	111.2
C7—C8—C10	112.7 (4)	H9D—C9'—H9F	109.0
C9—C8—C10	110.6 (4)	H9E—C9'—H9F	110.4
C7—C8—H8A	107.4	C8'—C10'—H10D	111.1
C9—C8—H8A	107.4	C8'—C10'—H10E	108.8
C10—C8—H8A	107.4	H10D—C10'—H10E	109.2
C8—C9—H9A	109.5	C8'—C10'—H10F	108.4
C8—C9—H9B	109.5	H10D—C10'—H10F	109.0
H9A—C9—H9B	109.5	H10E—C10'—H10F	110.3
C8—C9—H9C	109.5	C13'—C11'—C3'	112.7 (3)
H9A—C9—H9C	109.5	C13'—C11'—C12'	112.2 (4)
H9B—C9—H9C	109.5	C3'—C11'—C12'	113.0 (3)
C8—C10—H10A	109.5	C13'—C11'—H11B	106.1
C8—C10—H10B	109.5	C3'—C11'—H11B	106.1
H10A—C10—H10B	109.5	C12'—C11'—H11B	106.1
C8—C10—H10C	109.5	C11'—C12'—H12D	109.5
H10A—C10—H10C	109.5	C11'—C12'—H12E	109.5
H10B—C10—H10C	109.5	H12D—C12'—H12E	109.5
C13—C11—C3	113.5 (3)	C11'—C12'—H12F	109.5
C13—C11—C12	110.0 (3)	H12D—C12'—H12F	109.5
C3—C11—C12	109.5 (3)	H12E—C12'—H12F	109.5
C13—C11—H11A	107.9	C11'—C13'—H13D	109.5
C3—C11—H11A	107.9	C11'—C13'—H13E	109.5
C12—C11—H11A	107.9	H13D—C13'—H13E	109.5
C11—C12—H12A	109.5	C11'—C13'—H13F	109.5
C11—C12—H12B	109.5	H13D—C13'—H13F	109.5
H12A—C12—H12B	109.5	H13E—C13'—H13F	109.5
C11—C12—H12C	109.5

N1—C2—C3—C4	−176.8 (4)	C1'—N1'—C2'—C7'	−98 (2)
C7—C2—C3—C4	1.6 (7)	N1'—C2'—C3'—C4'	−176.2 (6)
N1—C2—C3—C11	1.8 (7)	C7'—C2'—C3'—C4'	1.0 (10)
C7—C2—C3—C11	−179.8 (5)	N1'—C2'—C3'—C11'	2.6 (9)
C2—C3—C4—C5	0.0 (8)	C7'—C2'—C3'—C11'	179.7 (6)
C11—C3—C4—C5	−178.5 (6)	C2'—C3'—C4'—C5'	−1.1 (10)
C3—C4—C5—C6	−2.0 (11)	C11'—C3'—C4'—C5'	−179.8 (8)
C4—C5—C6—C7	2.3 (13)	C3'—C4'—C5'—C6'	0.5 (14)
C5—C6—C7—C2	−0.6 (11)	C4'—C5'—C6'—C7'	0.3 (16)
C5—C6—C7—C8	179.8 (8)	C5'—C6'—C7'—C2'	−0.4 (13)
N1—C2—C7—C6	177.0 (6)	C5'—C6'—C7'—C8'	−178.6 (9)
C3—C2—C7—C6	−1.4 (8)	N1'—C2'—C7'—C6'	176.9 (7)
N1—C2—C7—C8	−3.4 (8)	C3'—C2'—C7'—C6'	−0.2 (10)
C3—C2—C7—C8	178.2 (6)	N1'—C2'—C7'—C8'	−4.9 (10)
C6—C7—C8—C9	101.3 (17)	C3'—C2'—C7'—C8'	178.0 (7)
C2—C7—C8—C9	−78.3 (17)	C6'—C7'—C8'—C9'	109 (2)
C6—C7—C8—C10	−23.5 (18)	C2'—C7'—C8'—C9'	−69 (2)
C2—C7—C8—C10	156.9 (18)	C6'—C7'—C8'—C10'	−15 (2)
C4—C3—C11—C13	22.5 (5)	C2'—C7'—C8'—C10'	167 (2)
C2—C3—C11—C13	−156.0 (5)	C4'—C3'—C11'—C13'	90.8 (5)
C4—C3—C11—C12	−100.8 (4)	C2'—C3'—C11'—C13'	−87.8 (6)
C2—C3—C11—C12	80.7 (5)	C4'—C3'—C11'—C12'	−37.7 (6)
C1'—N1'—C2'—C3'	79 (2)	C2'—C3'—C11'—C12'	143.7 (6)

Symmetry codes: (i) −x, −y, −z; (ii) y, −x+y, −z; (iii) −y, x−y, z; (iv) x−y, x, −z; (v) −x+y, −x, z.

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Niobium isocyanide com­plexes, Nb(CNAr)6, with Ar = 2,6-di­methyl­phenyl (X­yl), a diamagnetic dimer containing four reductively coupled isocyanides, and Ar = 2,6-diiso­propyl­phenyl (Dipp), a paramagnetic monomer analogous to the highly unstable hexa­carbonyl­niobium(0)

Supporting information

Niobium isocyanide complexes, Nb(CNAr)₆, with Ar = 2,6-dimethylphenyl (Xyl), a diamagnetic dimer containing four reductively coupled isocyanides, and Ar = 2,6-diisopropylphenyl (Dipp), a paramagnetic monomer analogous to the highly unstable hexacarbonylniobium(0)