A new double-cube nitride complex containing titanium and potassium

The reaction of the imide–nitride complex [{Ti(η⁵-C₅Me₅)(μ-NH)}₃(μ₃-N)] with potassium iodide in pyridine at room temperature affords the adduct di-μ-iodido-1:1′κ⁴I-bis­{tri-μ₃-imido-1:2:3κ³N;1:2:4κ³N;1:3:4κ³N-μ₃-nitrido-2:3:4κ³N-tris[2,3,4(η⁵)-penta­methyl­cyclo­penta­dien­yl](pyridine-1κN)-tetrahedro-potassiumtrititanium(IV)}, [K₂Ti₆(C₁₀H₁₅)₆I₂N₂(NH)₆(C₅H₅N)₂] or [(C₅H₅N)(μ-I)K{(μ₃-NH)₃Ti₃(η⁵-C₅Me₅)₃(μ₃-N)}]₂. The crystal structure contains two [KTi₃N₄] cube-type units held together by two bridging I atoms. There is a centre of inversion located in the middle of this unprecedented discrete K₂I₂ unit. The geometry around K is best described as distorted trigonal prismatic, with three imide groups, two bridging I atoms and one pyridine ligand.

S1. Comment

Polynuclear transition metal nitride complexes exhibit singular structures. These compounds might be of interest as building blocks in the synthesis of metal nitride materials (Oyama, 1996) or as intermediates in dinitrogen fixation and activation processes (see, for example, Fryzuk & Johnson, 2000; Himmel & Reiher, 2006; Kozak & Mountford, 2004). However, a review of the literature reveals a lack of a systematic synthetic method for the preparation of these polynuclear complexes (Abarca et al., 2003; Dehnicke & Strähle, 1992). In this context, the titanium imide–nitride compound [{Ti(η⁵-C₅Me₅)(µ-NH)}₃(µ₃-N)], (I) (Abarca et al., 2000; Roesky et al., 1989), is able to incorporate metal centres, and we have extensively investigated the rational synthesis of a series of heterometallic nitride complexes with cube-type structures. In particular, ligand (I) entraps alkali metal halides to give stable molecular adducts [XM{(µ₃-NH)₃Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}] (M = Li and X = Br, I; M = Na and X = I) (García-Castro et al., 2005). However, the analogous treatment of (I) with amides of group 1 elements affords edge-linked [M(µ₄-N)(µ₃-NH)₂{Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}]₂ or corner-shared [M(µ₃-N)(µ₃-NH)₅{Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}₂] double-cube complexes, depending on the reagent ratio of (I) and the amide (viz. 1:1 or 2:1; Martín et al., 2004).

The reaction of these edge-linked double-cube derivatives with metal halides has been used to prepare new heterometallic nitride complexes (García-Castro et al., 2001). Over the course of these investigations, we attempted to synthesize a zinc double-cube compound by treatment of the potassium derivative with ZnI₂ in pyridine. After three days at room temperature, yellow crystals of [(C₅H₅N)(µ-I)K{(µ₃-NH)₃Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}]₂, (II), were obtained in 27% yield. These crystals had a hexagonal prism shape and were air sensitive. Complex (II) was characterized by X-ray crystal structure determination, IR spectroscopy and CHN microanalysis. Compound (II) is not soluble in pyridine-d₅, and decomposes in benzene-d₆ or chloroform-d₁ to afford the imide–nitride ligand (I), KI and pyridine, precluding its characterization by NMR spectroscopy. Furthermore, a rational synthesis by reaction of (I) with KI in pyridine gave compound (II) in 73% yield.

The structure of (II) (Fig. 1) contains two [KTi₃N₄] cube-type units linked by two bridging I atoms and related by a centre of symmetry located in the middle of the planar K₂I₂ unit. The distance between the two K atoms is 4.629 (2) Å, clearly shorter than the K···K lengths found for [K₆I₄(dmp)₈]²⁺ [dmp is 2,9-dimethyl-1,10-phenanthroline; 4.960 (1) and 5.010 (1) Å], in which three K₂I₂ fragments are held together (Buttery et al., 2006). This phenanthroline derivative is the only compound in the Cambridge Structural Database (CSD, Version 5.32; Allen, 2002) containing I-bridged K₂I₂ units. Complexes with this type of unit, viz. M₂I₂, are common for the lighter alkali metal iodide complexes (see, for example, Barrett et al., 2006; Fei et al., 2003; Herberich et al., 2005) but, to the best of our knowledge, there are no structural examples of compounds with discrete K₂I₂ units. The K—I bond lengths in (II) [3.553 (1) and 3.605 (1) Å] are slightly longer than the values found for the phenanthroline complex [3.303 (1)–3.581 (1) Å]. The I—K—Iⁱ and K—I—Kⁱ angles [symmetry code: (i) -x + 1, -y + 1, -z + 2] in our discrete unit [99.39 (3) and 80.61 (3)°, respectively] are quite different to the values found for the polynuclear [K₆I₄(dmp)₈]²⁺ cation described by Buttery et al. (2006) [I—K—I = 85.78 (3)–88.77 (3)° and K—I—K = 89.23 (3)–97.39 (3)°].

The geometry around the potassium centre of (II) is best described as distorted trigonal prismatic, with the three imide groups of (I), two bridging iodide ligands and one N atom of the pyridine group occupying the six coordination positions. The K—N bond lengths [2.962 (3)–3.089 (3) Å] are similar to those found for potassium complexes containing the neutral tridentate ligand N,N,N',N'',N''-pentamethyldiethylenetriamine [2.838 (3)–3.066 (5) Å; Althaus et al., 1999; Craig et al., 1996; Fanjul et al., 2007]. Additionally, the K—N bond distances for (II) are longer than those found for the corner-shared double-cube complex [K(µ₃-N)(µ₃-NH)₅{Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}₂] [2.958 (2) Å; Martín et al., 2004] which presents intracube N—K—N angles [average 62.0 (1)°] very similar to those in (II) [60.70 (9)–62.09 (9)°]. The N_imide—K—I and N_imide—K—N_pyridine angles are in the range 74.18 (6)–138.2 (1)°, whereas the N_pyridine—K—I angles are 92.89 (9) and 124.17 (8)°. The K—N_pyridine bond length [2.896 (4) Å] compares well with those found in other potassium complexes containing a pyridine ligand [2.776 (3)–2.926 (2) Å; for example, Boyle et al., 2003].

The Ti—N1 and Ti—N_imide distances [average 1.939 (4) and 1.946 (5) Å, respectively] are slightly longer than those determined for the free ligand [1.913 (8) and 1.929 (8) Å; Roesky et al., 1989] and close to those found for the potassium corner-shared double-cube [1.928 (2) and 1.932 (6) Å; Martín et al., 2004]. The average N_imide—Ti—N_imide angle [104.0 (1)°] is similar to that observed in the potassium double-cube [104.1 (1)°], whereas it is narrower than the same angle in the structure of (I) [107.5 (7)°]. The remainder of the parameters within the tridentate organometallic ligand are similar to these cited complexes.

Related literature

For related literature, see: Abarca et al. (2000, 2003); Allen (2002); Althaus et al. (1999); Barrett et al. (2006); Boyle et al. (2003); Buttery et al. (2006); Craig et al. (1996); Dehnicke & Strähle (1992); Fanjul et al. (2007); Fei et al. (2003); Fryzuk & Johnson (2000); García-Castro, Gracia, Martín, Mena, Poblet, Sarasa & Yélamos (2005); García-Castro, Martín, Mena, Pérez-Redondo & Yélamos (2001); Herberich et al. (2005); Himmel & Reiher (2006); Kozak & Mountford (2004); Martín et al. (2004); Oyama (1996); Roesky et al. (1989).

S2. Experimental

All manipulations were carried out under an argon atmosphere using Schlenk line or glove-box techniques. Pyridine was distilled from CaH₂. Oven-dried glassware was repeatedly evacuated with a pumping system (ca 10 ^-3 Torr; 1 Torr = 133.322 Pa) and subsequently filled with inert gas. Samples for IR spectroscopy were prepared as KBr pellets. Microanalysis (CHN) was performed in a Leco CHNS-932 microanalyser.

[{Ti(η⁵-C₅Me₅)(µ-NH)}₃(µ₃-N)], (I), and [K(µ₄-N)(µ₃-NH)₂{Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}]₂ were prepared according to the methods of Abarca et al. (2000) and García-Castro et al. (2001), respectively. A pyridine solution (15 ml) of [K(µ₄-N)(µ₃-NH)₂{Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}]₂ (0.20 g, 0.15 mmol) was carefully layered with a pyridine solution (5 ml) of ZnI₂ (0.049 g, 0.15 mmol; Aldrich). The system was allowed to equilibrate for 3 d to afford yellow crystals of [(C₅H₅N)(µ-I)K{(µ₃-NH)₃Ti₃(η⁵-C₅Me₅)₃(µ₃-N)}]₂, (II) (yield 0.070 g, 27%). The following rational method of synthesis may also be employed. A 100 ml Schlenk flask was charged with (I) (0.30 g, 0.49 mmol), KI (0.080 g, 0.48 mmol; 98%, Aldrich) and pyridine (20 ml). The reaction mixture was stirred at room temperature for 20 h. The resultant pale-yellow solid was isolated by filtration, washed with pyridine (5 ml) and vacuum dried for 3 h to give (II) (yield 0.30 g, 73%). Spectroscopic analysis: IR (KBr, ν, cm^-1): 3315 (w), 2907 (m), 2855 (m), 1602 (w), 1584 (m), 1484 (w), 1438 (m), 1376 (m), 1218 (w), 1147 (w), 1069 (w), 1029 (m), 992 (w), 758 (vs), 713 (s), 676 (vs), 661 (vs), 643 (s), 606 (m), 575 (s), 472 (m), 423 (m). Analysis, calculated for C₇₀H₁₀₆I₂K₂N₁₀Ti₆: C 49.26, H 6.26, N 8.21%; found: C 49.62, H 6.56, N 8.13%.

S3. Refinement

H atoms bonded to C atoms were introduced at calculated positions and refined using a riding model, with C—H = 0.96 Å and U_iso(H) = 1.5U_eq(C) for methyl groups of the cyclopentadienyl rings, and with C—H = 0.93 Å and U_iso(H) = 1.2U_eq(C) for the pyridine ligand. The H atoms of the imide groups were found in an electron-density difference Fourier map at the final stages of the refinement procedure and were refined freely.

Computing details

Data collection: COLLECT (Nonius, 1998); cell refinement: DIRAX/LSQ (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures

Fig. 1. A perspective view of the molecule of (II), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry code: (i) -x + 1, -y + 1, -z + 2.]

di-µ-iodido-1:1'κ⁴I-bis[tri-µ₃-imido-1:2:3κ³N; 1:2:4κ³N;1:3:4κ³N-µ₃-nitrido-2:3:4κ³N- tris[2,3,4(η⁵)-pentamethylcyclopentadienyl](pyridine-1κN)- tetrahedro-potassiumtrititanium(IV)]

Crystal data

[K2Ti6(C10H15)6I2N2(NH)6(C5H5N)2]	Z = 1
Mr = 1707.05	F(000) = 872
Triclinic, P1	Dx = 1.38 Mg m^−3
a = 11.298 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.346 (2) Å	Cell parameters from 82 reflections
c = 18.391 (3) Å	θ = 3–19°
α = 101.66 (1)°	µ = 1.45 mm^−1
β = 93.46 (1)°	T = 200 K
γ = 115.55 (1)°	Prism, yellow
V = 2053.8 (6) Å^3	0.32 × 0.29 × 0.23 mm

Data collection

Nonius KappaCCD area-detector diffractometer	9150 independent reflections
Radiation source: Enraf–Nonius FR590	6034 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.045
Detector resolution: 9 pixels mm^-1	θmax = 27.5°, θmin = 3.3°
CCD rotation images, thick slices scans	h = −14→14
Absorption correction: multi-scan (Blessing, 1995)	k = −14→14
Tmin = 0.594, Tmax = 0.827	l = −23→23
34701 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.119	H atoms treated by a mixture of independent and constrained refinement
S = 0.98	w = 1/[σ^2(Fo^2) + (0.0609P)^2 + 0.0977P] where P = (Fo^2 + 2Fc^2)/3
9150 reflections	(Δ/σ)max = 0.002
433 parameters	Δρmax = 1.10 e Å^−3
0 restraints	Δρmin = −0.82 e Å^−3

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
C11	0.6813 (3)	0.4029 (4)	0.7540 (2)	0.0320 (8)
C12	0.7232 (3)	0.5237 (4)	0.8121 (2)	0.0318 (8)
C13	0.7454 (3)	0.6325 (4)	0.7784 (2)	0.0372 (9)
C14	0.7148 (4)	0.5777 (5)	0.6979 (2)	0.0409 (10)
C15	0.6754 (4)	0.4365 (5)	0.6832 (2)	0.0387 (10)
C16	0.6534 (4)	0.2661 (4)	0.7661 (3)	0.0461 (10)
H16A	0.5974	0.1969	0.7222	0.069*
H16B	0.6095	0.2531	0.809	0.069*
H16C	0.7358	0.2614	0.7747	0.069*
C17	0.7442 (4)	0.5378 (5)	0.8963 (2)	0.0449 (10)
H17A	0.6839	0.4552	0.907	0.067*
H17B	0.7279	0.6105	0.922	0.067*
H17C	0.8341	0.5565	0.913	0.067*
C18	0.7979 (4)	0.7789 (4)	0.8214 (3)	0.0557 (13)
H18A	0.7801	0.8284	0.7893	0.084*
H18B	0.8921	0.8172	0.8377	0.084*
H18C	0.7547	0.7837	0.8645	0.084*
C19	0.7303 (5)	0.6565 (6)	0.6384 (3)	0.0693 (16)
H19A	0.7254	0.7386	0.6591	0.104*
H19B	0.6605	0.603	0.596	0.104*
H19C	0.815	0.6776	0.6225	0.104*
C20	0.6413 (5)	0.3402 (6)	0.6067 (3)	0.0648 (15)
H20A	0.5839	0.2502	0.6097	0.097*
H20B	0.7214	0.3432	0.5903	0.097*
H20C	0.5968	0.3658	0.5714	0.097*
C21	0.2430 (4)	0.6774 (4)	0.6522 (2)	0.0345 (9)
C22	0.3768 (4)	0.7727 (4)	0.6849 (3)	0.0402 (10)
C23	0.3836 (4)	0.8151 (4)	0.7622 (3)	0.0453 (11)
C24	0.2547 (5)	0.7484 (5)	0.7798 (2)	0.0482 (11)
C25	0.1666 (4)	0.6633 (4)	0.7118 (3)	0.0411 (10)
C26	0.1911 (6)	0.6104 (6)	0.5688 (3)	0.0729 (16)
H26A	0.1	0.5438	0.562	0.109*
H26B	0.2437	0.5676	0.549	0.109*
H26C	0.197	0.6773	0.5426	0.109*
C27	0.4903 (5)	0.8189 (6)	0.6401 (4)	0.0812 (19)
H27A	0.487	0.7419	0.6051	0.122*
H27B	0.5738	0.8644	0.6739	0.122*
H27C	0.4816	0.8796	0.613	0.122*
C28	0.5051 (6)	0.9221 (5)	0.8196 (4)	0.089 (2)
H28A	0.5033	0.8964	0.8664	0.133*
H28B	0.5035	1.0076	0.8277	0.133*
H28C	0.5849	0.9294	0.8009	0.133*
C29	0.2150 (8)	0.7675 (7)	0.8581 (3)	0.098 (2)
H29A	0.1258	0.6999	0.8562	0.147*
H29B	0.2193	0.8555	0.8735	0.147*
H29C	0.2749	0.7589	0.8936	0.147*
C30	0.0164 (5)	0.5809 (6)	0.7021 (4)	0.082 (2)
H30A	−0.008	0.5628	0.7492	0.124*
H30B	−0.0115	0.4972	0.665	0.124*
H30C	−0.026	0.6308	0.686	0.124*
C31	0.1070 (4)	0.0565 (4)	0.6827 (2)	0.0396 (10)
C32	0.1903 (4)	0.0680 (4)	0.6273 (2)	0.0351 (9)
C33	0.1578 (4)	0.1316 (4)	0.5758 (2)	0.0429 (10)
C34	0.0503 (4)	0.1561 (4)	0.5985 (3)	0.0485 (12)
C35	0.0190 (4)	0.1097 (4)	0.6646 (3)	0.0466 (11)
C36	0.1103 (6)	−0.0070 (5)	0.7477 (3)	0.0707 (16)
H36A	0.0706	0.0247	0.7868	0.106*
H36B	0.2009	0.0177	0.7671	0.106*
H36C	0.0615	−0.1035	0.7301	0.106*
C37	0.2952 (5)	0.0175 (5)	0.6239 (3)	0.0650 (15)
H37A	0.3373	0.0348	0.5807	0.098*
H37B	0.2537	−0.0778	0.6199	0.098*
H37C	0.3608	0.0637	0.6688	0.098*
C38	0.2226 (7)	0.1628 (5)	0.5072 (3)	0.083 (2)
H38A	0.3011	0.1498	0.5092	0.124*
H38B	0.2463	0.2548	0.507	0.124*
H38C	0.1611	0.1036	0.4622	0.124*
C39	−0.0204 (7)	0.2174 (5)	0.5573 (4)	0.106 (3)
H39A	−0.0533	0.2654	0.5928	0.159*
H39B	−0.0934	0.1468	0.5206	0.159*
H39C	0.041	0.2786	0.5325	0.159*
C40	−0.0917 (5)	0.1113 (6)	0.7073 (4)	0.090 (2)
H40A	−0.0654	0.1221	0.7598	0.134*
H40B	−0.1711	0.0278	0.6879	0.134*
H40C	−0.1086	0.1851	0.7013	0.134*
N1	0.3709 (3)	0.4524 (3)	0.66719 (16)	0.0276 (6)
N12	0.4739 (3)	0.6157 (3)	0.80365 (17)	0.0267 (6)
N13	0.3862 (3)	0.3109 (3)	0.76297 (18)	0.0295 (7)
N23	0.1795 (3)	0.4169 (3)	0.74969 (17)	0.0295 (7)
Ti1	0.51229 (6)	0.47830 (6)	0.74308 (3)	0.02487 (15)
Ti2	0.32196 (6)	0.57712 (6)	0.73130 (3)	0.02383 (15)
Ti3	0.24024 (6)	0.29469 (6)	0.69314 (4)	0.02655 (15)
K1	0.33000 (8)	0.44731 (9)	0.90362 (5)	0.0383 (2)
I1	0.43572 (3)	0.23225 (3)	0.973406 (16)	0.04420 (11)
H12	0.527 (4)	0.689 (4)	0.839 (2)	0.028 (10)*
H13	0.404 (4)	0.259 (5)	0.778 (2)	0.044 (14)*
H23	0.105 (4)	0.397 (4)	0.757 (2)	0.047 (14)*
C102	−0.0438 (5)	0.3309 (5)	0.9240 (3)	0.0583 (13)
H102	−0.0299	0.4113	0.9122	0.07*
C103	−0.1669 (5)	0.2515 (6)	0.9407 (3)	0.0642 (15)
H103	−0.2333	0.2791	0.9402	0.077*
C104	−0.1901 (5)	0.1318 (5)	0.9579 (3)	0.0577 (13)
H104	−0.2722	0.0772	0.969	0.069*
C105	−0.0890 (5)	0.0945 (5)	0.9583 (3)	0.0568 (13)
H105	−0.102	0.0141	0.9698	0.068*
C106	0.0319 (5)	0.1780 (5)	0.9414 (3)	0.0556 (12)
H106	0.099	0.1513	0.9417	0.067*
N101	0.0579 (4)	0.2964 (4)	0.9243 (2)	0.0526 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C11	0.0298 (19)	0.037 (2)	0.037 (2)	0.0223 (17)	0.0044 (15)	0.0096 (17)
C12	0.0239 (18)	0.037 (2)	0.036 (2)	0.0152 (16)	0.0014 (15)	0.0094 (17)
C13	0.0229 (18)	0.038 (2)	0.055 (3)	0.0146 (16)	0.0103 (16)	0.0168 (19)
C14	0.033 (2)	0.059 (3)	0.046 (3)	0.027 (2)	0.0193 (17)	0.029 (2)
C15	0.030 (2)	0.059 (3)	0.036 (2)	0.0264 (19)	0.0110 (16)	0.013 (2)
C16	0.048 (2)	0.044 (3)	0.056 (3)	0.031 (2)	0.006 (2)	0.012 (2)
C17	0.048 (2)	0.054 (3)	0.037 (2)	0.028 (2)	−0.0016 (18)	0.010 (2)
C18	0.036 (2)	0.032 (2)	0.092 (4)	0.0090 (19)	0.010 (2)	0.016 (2)
C19	0.058 (3)	0.106 (5)	0.083 (4)	0.050 (3)	0.034 (3)	0.069 (4)
C20	0.062 (3)	0.101 (4)	0.042 (3)	0.051 (3)	0.014 (2)	0.005 (3)
C21	0.044 (2)	0.030 (2)	0.040 (2)	0.0264 (18)	0.0023 (17)	0.0119 (17)
C22	0.045 (2)	0.036 (2)	0.058 (3)	0.0268 (19)	0.0155 (19)	0.029 (2)
C23	0.056 (3)	0.018 (2)	0.058 (3)	0.0177 (18)	−0.012 (2)	0.0056 (19)
C24	0.084 (3)	0.043 (3)	0.044 (3)	0.049 (3)	0.023 (2)	0.018 (2)
C25	0.034 (2)	0.034 (2)	0.072 (3)	0.0254 (18)	0.016 (2)	0.025 (2)
C26	0.117 (5)	0.062 (3)	0.051 (3)	0.055 (3)	−0.011 (3)	0.011 (3)
C27	0.077 (4)	0.084 (4)	0.135 (6)	0.054 (3)	0.063 (4)	0.083 (4)
C28	0.103 (4)	0.028 (3)	0.105 (5)	0.023 (3)	−0.051 (4)	−0.010 (3)
C29	0.194 (7)	0.104 (5)	0.066 (4)	0.117 (5)	0.066 (4)	0.039 (4)
C30	0.039 (3)	0.058 (3)	0.169 (7)	0.028 (3)	0.024 (3)	0.052 (4)
C31	0.044 (2)	0.0203 (19)	0.041 (2)	0.0038 (17)	−0.0006 (18)	0.0072 (17)
C32	0.044 (2)	0.0186 (18)	0.039 (2)	0.0134 (16)	0.0027 (17)	0.0029 (16)
C33	0.057 (3)	0.022 (2)	0.031 (2)	0.0055 (19)	−0.0064 (18)	0.0011 (17)
C34	0.046 (2)	0.023 (2)	0.061 (3)	0.0114 (18)	−0.026 (2)	−0.001 (2)
C35	0.031 (2)	0.025 (2)	0.065 (3)	0.0051 (17)	0.0008 (19)	−0.007 (2)
C36	0.088 (4)	0.038 (3)	0.067 (3)	0.007 (3)	0.002 (3)	0.026 (3)
C37	0.068 (3)	0.037 (3)	0.085 (4)	0.031 (2)	0.003 (3)	−0.009 (3)
C38	0.124 (5)	0.048 (3)	0.040 (3)	0.007 (3)	0.009 (3)	0.010 (2)
C39	0.110 (5)	0.040 (3)	0.135 (6)	0.029 (3)	−0.085 (4)	−0.004 (3)
C40	0.034 (3)	0.058 (4)	0.139 (6)	0.006 (2)	0.019 (3)	−0.021 (4)
N1	0.0357 (16)	0.0263 (16)	0.0248 (16)	0.0165 (13)	0.0069 (12)	0.0086 (13)
N12	0.0269 (15)	0.0207 (16)	0.0300 (17)	0.0100 (13)	0.0028 (12)	0.0036 (13)
N13	0.0333 (17)	0.0279 (17)	0.0328 (18)	0.0169 (14)	0.0040 (13)	0.0127 (14)
N23	0.0274 (17)	0.0266 (17)	0.0369 (18)	0.0128 (14)	0.0080 (13)	0.0112 (14)
Ti1	0.0254 (3)	0.0251 (3)	0.0292 (3)	0.0145 (3)	0.0063 (2)	0.0097 (3)
Ti2	0.0257 (3)	0.0192 (3)	0.0291 (3)	0.0120 (3)	0.0033 (2)	0.0076 (3)
Ti3	0.0287 (3)	0.0189 (3)	0.0311 (4)	0.0110 (3)	0.0007 (3)	0.0052 (3)
K1	0.0436 (5)	0.0413 (5)	0.0328 (5)	0.0186 (4)	0.0104 (4)	0.0156 (4)
I1	0.05457 (19)	0.03754 (17)	0.04513 (18)	0.02405 (14)	0.00893 (12)	0.01264 (12)
C102	0.067 (3)	0.059 (3)	0.058 (3)	0.031 (3)	0.011 (2)	0.028 (3)
C103	0.061 (3)	0.100 (5)	0.051 (3)	0.051 (3)	0.010 (2)	0.025 (3)
C104	0.044 (3)	0.066 (3)	0.043 (3)	0.007 (2)	0.005 (2)	0.016 (2)
C105	0.069 (3)	0.039 (3)	0.046 (3)	0.013 (2)	−0.003 (2)	0.007 (2)
C106	0.055 (3)	0.057 (3)	0.059 (3)	0.034 (3)	0.002 (2)	0.007 (3)
N101	0.052 (2)	0.059 (3)	0.044 (2)	0.020 (2)	0.0070 (17)	0.0166 (19)

Geometric parameters (Å, º)

K1—N12	2.962 (3)	C25—C30	1.521 (6)
K1—N13	2.986 (3)	C25—Ti2	2.390 (4)
K1—N23	3.089 (3)	C26—H26A	0.96
K1—N101	2.896 (4)	C26—H26B	0.96
K1—I1	3.553 (1)	C26—H26C	0.96
K1—I1^i	3.605 (1)	C27—H27A	0.96
Ti1—N12	1.949 (3)	C27—H27B	0.96
Ti1—N13	1.944 (3)	C27—H27C	0.96
Ti2—N12	1.936 (3)	C28—H28A	0.96
Ti2—N23	1.950 (3)	C28—H28B	0.96
Ti3—N13	1.947 (3)	C28—H28C	0.96
Ti3—N23	1.949 (3)	C29—H29A	0.96
Ti1—N1	1.936 (3)	C29—H29B	0.96
Ti2—N1	1.943 (3)	C29—H29C	0.96
Ti3—N1	1.939 (3)	C30—H30A	0.96
I1—K1^i	3.6046 (12)	C30—H30B	0.96
C11—C12	1.426 (5)	C30—H30C	0.96
C11—C15	1.434 (5)	C31—C32	1.416 (6)
C11—C16	1.511 (6)	C31—C35	1.422 (6)
C11—Ti1	2.420 (3)	C31—C36	1.521 (6)
C12—C13	1.427 (6)	C31—Ti3	2.419 (4)
C12—C17	1.516 (5)	C32—C33	1.419 (6)
C12—Ti1	2.423 (3)	C32—C37	1.523 (6)
C13—C14	1.441 (6)	C32—Ti3	2.410 (4)
C13—C18	1.516 (6)	C33—C34	1.426 (6)
C13—Ti1	2.404 (4)	C33—C38	1.524 (7)
C14—C15	1.426 (6)	C33—Ti3	2.367 (4)
C14—C19	1.520 (6)	C34—C35	1.425 (7)
C14—Ti1	2.362 (4)	C34—C39	1.521 (6)
C15—C20	1.507 (6)	C34—Ti3	2.375 (4)
C15—Ti1	2.371 (4)	C35—C40	1.522 (7)
C16—H16A	0.96	C35—Ti3	2.408 (4)
C16—H16B	0.96	C36—H36A	0.96
C16—H16C	0.96	C36—H36B	0.96
C17—H17A	0.96	C36—H36C	0.96
C17—H17B	0.96	C37—H37A	0.96
C17—H17C	0.96	C37—H37B	0.96
C18—H18A	0.96	C37—H37C	0.96
C18—H18B	0.96	C38—H38A	0.96
C18—H18C	0.96	C38—H38B	0.96
C19—H19A	0.96	C38—H38C	0.96
C19—H19B	0.96	C39—H39A	0.96
C19—H19C	0.96	C39—H39B	0.96
C20—H20A	0.96	C39—H39C	0.96
C20—H20B	0.96	C40—H40A	0.96
C20—H20C	0.96	C40—H40B	0.96
C21—C25	1.428 (6)	C40—H40C	0.96
C21—C22	1.426 (6)	C102—N101	1.364 (6)
C21—C26	1.520 (6)	C102—C103	1.386 (7)
C21—Ti2	2.366 (4)	C102—H102	0.93
C22—C23	1.391 (6)	C103—C104	1.375 (8)
C22—C27	1.524 (6)	C103—H103	0.93
C22—Ti2	2.383 (4)	C104—C105	1.378 (7)
C23—C24	1.416 (6)	C104—H104	0.93
C23—C28	1.531 (6)	C105—C106	1.384 (7)
C23—Ti2	2.410 (4)	C105—H105	0.93
C24—C25	1.422 (6)	C106—N101	1.353 (6)
C24—C29	1.535 (7)	C106—H106	0.93
C24—Ti2	2.410 (4)
N12—K1—N13	62.09 (9)	C34—C39—H39B	109.5
N12—K1—N23	60.70 (9)	H39A—C39—H39B	109.5
N13—K1—N23	60.71 (9)	C34—C39—H39C	109.5
N12—K1—I1	123.11 (6)	H39A—C39—H39C	109.5
N12—K1—I1^i	74.18 (6)	H39B—C39—H39C	109.5
N12—K1—N101	138.2 (1)	C35—C40—H40A	109.5
N13—K1—I1	79.45 (7)	C35—C40—H40B	109.5
N13—K1—I1^i	124.46 (7)	H40A—C40—H40B	109.5
N13—K1—N101	111.3 (1)	C35—C40—H40C	109.5
N23—K1—I1	132.43 (7)	H40A—C40—H40C	109.5
N23—K1—I1^i	123.68 (6)	H40B—C40—H40C	109.5
N23—K1—N101	79.8 (1)	N1—Ti1—C14	107.54 (13)
N101—K1—I1	92.89 (9)	N13—Ti1—C14	142.90 (15)
N101—K1—I1^i	124.17 (8)	N12—Ti1—C14	111.06 (15)
I1—K1—I1^i	99.39 (3)	N1—Ti1—C15	109.24 (13)
K1—I1—K1^i	80.61 (3)	N13—Ti1—C15	108.10 (15)
N12—Ti1—N13	104.0 (1)	N12—Ti1—C15	145.14 (14)
N12—Ti2—N23	103.9 (1)	C14—Ti1—C15	35.07 (15)
N13—Ti3—N23	104.1 (1)	N1—Ti1—C13	134.66 (13)
N1—Ti1—N12	85.8 (1)	N13—Ti1—C13	138.27 (14)
N1—Ti1—N13	86.4 (1)	N12—Ti1—C13	88.70 (13)
N1—Ti2—N12	86.0 (1)	C14—Ti1—C13	35.19 (14)
N1—Ti2—N23	85.9 (1)	C15—Ti1—C13	58.10 (14)
N1—Ti3—N13	86.3 (1)	N1—Ti1—C11	137.95 (13)
N1—Ti3—N23	86.0 (1)	N13—Ti1—C11	88.39 (13)
Ti1—N1—Ti2	94.0 (1)	N12—Ti1—C11	135.74 (13)
Ti1—N1—Ti3	93.7 (1)	C14—Ti1—C11	57.97 (14)
Ti2—N1—Ti3	94.1 (1)	C15—Ti1—C11	34.83 (13)
Ti1—N12—Ti2	93.8 (1)	C13—Ti1—C11	57.46 (13)
Ti1—N12—K1	95.2 (1)	N1—Ti1—C12	165.05 (12)
Ti1—N12—H12	130 (2)	N13—Ti1—C12	103.92 (13)
Ti2—N12—K1	98.3 (1)	N12—Ti1—C12	101.79 (13)
Ti2—N12—H12	132 (2)	C14—Ti1—C12	57.79 (13)
K1—N12—H12	98 (2)	C15—Ti1—C12	57.57 (13)
Ti1—N13—Ti3	93.2 (1)	C13—Ti1—C12	34.39 (13)
Ti1—N13—K1	94.5 (1)	C11—Ti1—C12	34.26 (13)
Ti1—N13—H13	126 (3)	N1—Ti1—Ti3	43.20 (9)
Ti3—N13—K1	97.9 (1)	N13—Ti1—Ti3	43.43 (10)
Ti3—N13—H13	134 (3)	N12—Ti1—Ti3	93.33 (9)
K1—N13—H13	101 (3)	C14—Ti1—Ti3	141.62 (11)
Ti2—N23—Ti3	93.6 (1)	C15—Ti1—Ti3	119.41 (11)
Ti2—N23—K1	94.0 (1)	C13—Ti1—Ti3	176.81 (11)
Ti2—N23—H23	134 (3)	C11—Ti1—Ti3	121.97 (10)
Ti3—N23—K1	94.6 (1)	C12—Ti1—Ti3	146.96 (10)
Ti3—N23—H23	126 (3)	N1—Ti1—Ti2	43.09 (9)
K1—N23—H23	103 (3)	N13—Ti1—Ti2	93.70 (10)
C12—C11—C15	107.6 (3)	N12—Ti1—Ti2	42.92 (9)
C12—C11—C16	125.4 (4)	C14—Ti1—Ti2	120.24 (11)
C15—C11—C16	127.0 (4)	C15—Ti1—Ti2	144.51 (10)
C12—C11—Ti1	73.0 (2)	C13—Ti1—Ti2	120.33 (10)
C15—C11—Ti1	70.7 (2)	C11—Ti1—Ti2	177.79 (10)
C16—C11—Ti1	123.4 (3)	C12—Ti1—Ti2	144.08 (10)
C11—C12—C13	108.7 (3)	Ti3—Ti1—Ti2	60.22 (3)
C11—C12—C17	126.7 (4)	N1—Ti1—K1	98.39 (9)
C13—C12—C17	124.6 (4)	N13—Ti1—K1	53.79 (10)
C11—C12—Ti1	72.76 (19)	N12—Ti1—K1	53.10 (9)
C13—C12—Ti1	72.1 (2)	C14—Ti1—K1	148.83 (11)
C17—C12—Ti1	122.1 (2)	C15—Ti1—K1	146.36 (10)
C12—C13—C14	107.5 (4)	C13—Ti1—K1	113.64 (10)
C12—C13—C18	124.7 (4)	C11—Ti1—K1	111.70 (9)
C14—C13—C18	127.7 (4)	C12—Ti1—K1	96.44 (9)
C12—C13—Ti1	73.5 (2)	Ti3—Ti1—K1	69.54 (3)
C14—C13—Ti1	70.8 (2)	Ti2—Ti1—K1	69.09 (2)
C18—C13—Ti1	123.3 (3)	N12—Ti2—C21	141.77 (13)
C15—C14—C13	107.9 (3)	N1—Ti2—C21	107.24 (13)
C15—C14—C19	125.3 (4)	N23—Ti2—C21	112.55 (14)
C13—C14—C19	126.6 (4)	N12—Ti2—C22	106.91 (14)
C15—C14—Ti1	72.8 (2)	N1—Ti2—C22	110.02 (14)
C13—C14—Ti1	74.0 (2)	N23—Ti2—C22	146.05 (14)
C19—C14—Ti1	122.2 (3)	C21—Ti2—C22	34.96 (14)
C14—C15—C11	108.2 (3)	N12—Ti2—C25	139.28 (15)
C14—C15—C20	126.1 (4)	N1—Ti2—C25	133.84 (15)
C11—C15—C20	125.6 (4)	N23—Ti2—C25	89.61 (14)
C14—C15—Ti1	72.1 (2)	C21—Ti2—C25	34.94 (14)
C11—C15—Ti1	74.4 (2)	C22—Ti2—C25	57.50 (13)
C20—C15—Ti1	122.1 (3)	N12—Ti2—C23	88.62 (14)
C11—C16—H16A	109.5	N1—Ti2—C23	138.12 (15)
C11—C16—H16B	109.5	N23—Ti2—C23	135.51 (15)
H16A—C16—H16B	109.5	C21—Ti2—C23	57.35 (14)
C11—C16—H16C	109.5	C22—Ti2—C23	33.73 (15)
H16A—C16—H16C	109.5	C25—Ti2—C23	57.17 (14)
H16B—C16—H16C	109.5	N12—Ti2—C24	104.82 (15)
C12—C17—H17A	109.5	N1—Ti2—C24	164.61 (14)
C12—C17—H17B	109.5	N23—Ti2—C24	101.76 (15)
H17A—C17—H17B	109.5	C21—Ti2—C24	57.55 (14)
C12—C17—H17C	109.5	C22—Ti2—C24	56.71 (15)
H17A—C17—H17C	109.5	C25—Ti2—C24	34.46 (15)
H17B—C17—H17C	109.5	C23—Ti2—C24	34.17 (16)
C13—C18—H18A	109.5	N12—Ti2—Ti1	43.28 (9)
C13—C18—H18B	109.5	N1—Ti2—Ti1	42.90 (9)
H18A—C18—H18B	109.5	N23—Ti2—Ti1	93.21 (10)
C13—C18—H18C	109.5	C21—Ti2—Ti1	140.46 (10)
H18A—C18—H18C	109.5	C22—Ti2—Ti1	119.09 (10)
H18B—C18—H18C	109.5	C25—Ti2—Ti1	175.37 (11)
C14—C19—H19A	109.5	C23—Ti2—Ti1	122.22 (11)
C14—C19—H19B	109.5	C24—Ti2—Ti1	147.69 (12)
H19A—C19—H19B	109.5	N12—Ti2—Ti3	93.17 (9)
C14—C19—H19C	109.5	N1—Ti2—Ti3	42.90 (9)
H19A—C19—H19C	109.5	N23—Ti2—Ti3	43.21 (10)
H19B—C19—H19C	109.5	C21—Ti2—Ti3	121.19 (10)
C15—C20—H20A	109.5	C22—Ti2—Ti3	145.85 (11)
C15—C20—H20B	109.5	C25—Ti2—Ti3	120.88 (10)
H20A—C20—H20B	109.5	C23—Ti2—Ti3	178.05 (10)
C15—C20—H20C	109.5	C24—Ti2—Ti3	144.27 (12)
H20A—C20—H20C	109.5	Ti1—Ti2—Ti3	59.72 (2)
H20B—C20—H20C	109.5	N12—Ti2—K1	51.09 (9)
C25—C21—C22	107.1 (4)	N1—Ti2—K1	95.81 (9)
C25—C21—C26	126.8 (4)	N23—Ti2—K1	54.90 (9)
C22—C21—C26	126.0 (4)	C21—Ti2—K1	153.33 (10)
C25—C21—Ti2	73.4 (2)	C22—Ti2—K1	145.50 (11)
C22—C21—Ti2	73.2 (2)	C25—Ti2—K1	118.42 (11)
C26—C21—Ti2	121.5 (3)	C23—Ti2—K1	112.49 (11)
C23—C22—C21	108.9 (4)	C24—Ti2—K1	99.51 (11)
C23—C22—C27	127.2 (5)	Ti1—Ti2—K1	66.19 (2)
C21—C22—C27	123.9 (4)	Ti3—Ti2—K1	68.20 (3)
C23—C22—Ti2	74.2 (2)	N1—Ti3—C33	102.49 (13)
C21—C22—Ti2	71.9 (2)	N13—Ti3—C33	121.54 (15)
C27—C22—Ti2	120.6 (3)	N23—Ti3—C33	133.87 (15)
C22—C23—C24	108.4 (4)	N1—Ti3—C34	114.67 (15)
C22—C23—C28	127.4 (5)	N13—Ti3—C34	149.01 (14)
C24—C23—C28	124.1 (5)	N23—Ti3—C34	100.17 (15)
C22—C23—Ti2	72.1 (2)	C33—Ti3—C34	35.00 (16)
C24—C23—Ti2	72.9 (2)	N1—Ti3—C32	122.40 (13)
C28—C23—Ti2	124.0 (3)	N13—Ti3—C32	92.55 (14)
C23—C24—C25	108.1 (4)	N23—Ti3—C32	148.31 (14)
C23—C24—C29	126.4 (5)	C33—Ti3—C32	34.56 (14)
C25—C24—C29	125.5 (5)	C34—Ti3—C32	57.28 (14)
C23—C24—Ti2	72.9 (2)	N1—Ti3—C35	148.16 (15)
C25—C24—Ti2	72.0 (2)	N13—Ti3—C35	124.88 (16)
C29—C24—Ti2	122.3 (3)	N23—Ti3—C35	91.74 (14)
C24—C25—C21	107.6 (3)	C33—Ti3—C35	57.79 (16)
C24—C25—C30	126.9 (5)	C34—Ti3—C35	34.66 (16)
C21—C25—C30	125.4 (5)	C32—Ti3—C35	56.85 (14)
C24—C25—Ti2	73.5 (2)	N1—Ti3—C31	156.50 (14)
C21—C25—Ti2	71.6 (2)	N13—Ti3—C31	94.16 (14)
C30—C25—Ti2	124.3 (3)	N23—Ti3—C31	116.50 (14)
C21—C26—H26A	109.5	C33—Ti3—C31	57.55 (14)
C21—C26—H26B	109.5	C34—Ti3—C31	57.37 (14)
H26A—C26—H26B	109.5	C32—Ti3—C31	34.10 (14)
C21—C26—H26C	109.5	C35—Ti3—C31	34.26 (15)
H26A—C26—H26C	109.5	N1—Ti3—Ti1	43.11 (9)
H26B—C26—H26C	109.5	N13—Ti3—Ti1	43.35 (10)
C22—C27—H27A	109.5	N23—Ti3—Ti1	93.52 (10)
C22—C27—H27B	109.5	C33—Ti3—Ti1	123.62 (12)
H27A—C27—H27B	109.5	C34—Ti3—Ti1	153.18 (13)
C22—C27—H27C	109.5	C32—Ti3—Ti1	116.55 (10)
H27A—C27—H27C	109.5	C35—Ti3—Ti1	168.10 (12)
H27B—C27—H27C	109.5	C31—Ti3—Ti1	134.54 (11)
C23—C28—H28A	109.5	N1—Ti3—Ti2	43.00 (9)
C23—C28—H28B	109.5	N13—Ti3—Ti2	93.50 (10)
H28A—C28—H28B	109.5	N23—Ti3—Ti2	43.22 (10)
C23—C28—H28C	109.5	C33—Ti3—Ti2	131.53 (10)
H28A—C28—H28C	109.5	C34—Ti3—Ti2	117.45 (11)
H28B—C28—H28C	109.5	C32—Ti3—Ti2	163.59 (10)
C24—C29—H29A	109.5	C35—Ti3—Ti2	129.35 (11)
C24—C29—H29B	109.5	C31—Ti3—Ti2	159.66 (11)
H29A—C29—H29B	109.5	Ti1—Ti3—Ti2	60.06 (2)
C24—C29—H29C	109.5	N1—Ti3—K1	95.36 (9)
H29A—C29—H29C	109.5	N13—Ti3—K1	51.42 (10)
H29B—C29—H29C	109.5	N23—Ti3—K1	54.48 (9)
C25—C30—H30A	109.5	C33—Ti3—K1	160.53 (10)
C25—C30—H30B	109.5	C34—Ti3—K1	140.15 (13)
H30A—C30—H30B	109.5	C32—Ti3—K1	127.31 (10)
C25—C30—H30C	109.5	C35—Ti3—K1	109.04 (12)
H30A—C30—H30C	109.5	C31—Ti3—K1	103.25 (10)
H30B—C30—H30C	109.5	Ti1—Ti3—K1	66.02 (3)
C32—C31—C35	107.8 (4)	Ti2—Ti3—K1	67.58 (3)
C32—C31—C36	124.9 (4)	N101—K1—Ti1	136.19 (8)
C35—C31—C36	127.3 (4)	N12—K1—Ti1	31.75 (6)
C32—C31—Ti3	72.6 (2)	N13—K1—Ti1	31.69 (6)
C35—C31—Ti3	72.4 (2)	N23—K1—Ti1	62.05 (6)
C36—C31—Ti3	122.4 (3)	I1—K1—Ti1	97.43 (3)
C31—C32—C33	108.7 (4)	I1^i—K1—Ti1	95.95 (3)
C31—C32—C37	124.8 (4)	N101—K1—Ti2	107.91 (8)
C33—C32—C37	126.4 (4)	N12—K1—Ti2	30.57 (6)
C31—C32—Ti3	73.3 (2)	N13—K1—Ti2	61.99 (7)
C33—C32—Ti3	71.1 (2)	N23—K1—Ti2	31.09 (6)
C37—C32—Ti3	122.4 (3)	I1—K1—Ti2	140.55 (3)
C32—C33—C34	107.4 (4)	I1^i—K1—Ti2	95.99 (3)
C32—C33—C38	126.1 (5)	Ti1—K1—Ti2	44.717 (18)
C34—C33—C38	126.4 (5)	N101—K1—Ti3	91.75 (8)
C32—C33—Ti3	74.4 (2)	N12—K1—Ti3	61.62 (6)
C34—C33—Ti3	72.8 (2)	N13—K1—Ti3	30.64 (6)
C38—C33—Ti3	120.3 (3)	N23—K1—Ti3	30.90 (6)
C33—C34—C35	108.1 (4)	I1—K1—Ti3	103.91 (3)
C33—C34—C39	125.4 (5)	I1^i—K1—Ti3	135.79 (3)
C35—C34—C39	126.5 (5)	Ti1—K1—Ti3	44.441 (19)
C33—C34—Ti3	72.2 (2)	Ti2—K1—Ti3	44.217 (19)
C35—C34—Ti3	73.9 (2)	N101—K1—K1^i	118.42 (8)
C39—C34—Ti3	121.0 (3)	N12—K1—K1^i	101.95 (7)
C31—C35—C34	107.9 (4)	N13—K1—K1^i	107.45 (7)
C31—C35—C40	125.4 (5)	N23—K1—K1^i	161.73 (7)
C34—C35—C40	126.6 (5)	I1—K1—K1^i	50.19 (2)
C31—C35—Ti3	73.3 (2)	I1^i—K1—K1^i	49.21 (2)
C34—C35—Ti3	71.4 (2)	Ti1—K1—K1^i	100.37 (3)
C40—C35—Ti3	122.7 (3)	Ti2—K1—K1^i	132.37 (3)
C31—C36—H36A	109.5	Ti3—K1—K1^i	137.95 (4)
C31—C36—H36B	109.5	N101—C102—C103	123.0 (5)
H36A—C36—H36B	109.5	N101—C102—H102	118.5
C31—C36—H36C	109.5	C103—C102—H102	118.5
H36A—C36—H36C	109.5	C104—C103—C102	119.6 (5)
H36B—C36—H36C	109.5	C104—C103—H103	120.2
C32—C37—H37A	109.5	C102—C103—H103	120.2
C32—C37—H37B	109.5	C103—C104—C105	118.5 (4)
H37A—C37—H37B	109.5	C103—C104—H104	120.7
C32—C37—H37C	109.5	C105—C104—H104	120.7
H37A—C37—H37C	109.5	C106—C105—C104	119.3 (5)
H37B—C37—H37C	109.5	C106—C105—H105	120.4
C33—C38—H38A	109.5	C104—C105—H105	120.4
C33—C38—H38B	109.5	N101—C106—C105	123.6 (5)
H38A—C38—H38B	109.5	N101—C106—H106	118.2
C33—C38—H38C	109.5	C105—C106—H106	118.2
H38A—C38—H38C	109.5	C106—N101—C102	116.0 (4)
H38B—C38—H38C	109.5	C106—N101—K1	114.1 (3)
C34—C39—H39A	109.5	C102—N101—K1	129.7 (3)

Symmetry code: (i) −x+1, −y+1, −z+2.