research papers\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoSTRUCTURAL
CHEMISTRY
ISSN: 2053-2296

Coordination variety of phenyl­tetra­zolato and di­methyl­amido ligands in dimeric Ti, Zr, and Ta com­plexes

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aDepartment of Chemistry, University of Wisconsin-Madison, 1101 University Ave, Madison, WI 53706, USA
*Correspondence e-mail: iguzei@chem.wisc.edu

Edited by A. Lemmerer, University of the Witwatersrand, South Africa (Received 21 June 2024; accepted 26 July 2024; online 23 August 2024)

Three structurally diverse 5-phenyl­tetra­zolato (Tz) Ti, Zr, and Ta com­plexes, namely, (C2H8N)[Ti2(C7H5N4)5(C2H6N)4]·1.45C6H6 or (Me2NH2)[Ti2(NMe2)4(2,3-μ-Tz)3(2-η1-Tz)2]·1.45C6H6, (1·1.45C6H6), [Zr2(C7H5N4)6(C2H6N)2(C2H7N)2]·1.12C6H6·0.382CH2Cl2 or [Zr2(Me2NH)2(NMe2)2(2,3-μ-Tz)3(2-η1-Tz)2(1,2-η2-Tz)]·1.12C6H6·0.38CH2Cl2 (2·1.12C6H6·0.38CH2Cl2), and (C2H8N)2[Ta2(C7H5N4)8(C2H6N)2O]·0.25C7H8 or (Me2NH2)2[Ta2(NMe2)2(2,3-μ-Tz)2(2-η1-Tz)6O]·0.25C7H8 (3·0.25C7H8), where TzH is 5-phenyl-1H-tetra­zole, have been synthesized and structurally characterized. All three com­plexes are dinuclear; the Ti center in 1 is six-coordinate, whereas the Zr and Ta atoms in 2 and 3 are seven-coordinate. The coordination environments of the Ti centers in 1 are similar, and so are the ligations of the Ta centers in 3. In contrast, the two Zr centers in 2 bear a different number of ligands, one of which is a bidentate η2-5-phenyl­tetra­zolato ligand that has not been observed previously for d-block elements. The di­methyl­amido ligand, present in the starting materials, remained un­changed, or was converted to di­methyl­amine and di­methyl­ammonium during the synthesis. Di­methyl­amine coordinates as a neutral ligand, whereas di­methyl­ammonium is retained as a hy­dro­gen-bonded entity bridging Tz ligands.

1. Introduction

Since the discovery of a facile synthesis of stable com­plexes of d-block elements with η2-coordinated pyrazoles (Guzei et al., 1997[Guzei, I. A., Baboul, A. G., Yap, G. P. A., Rheingold, A. L., Schlegel, H. B. & Winter, C. H. (1997). J. Am. Chem. Soc. 119, 3387-3388.]), we have been inter­ested in the preparation of transition-metal com­plexes with similarly coordinated 5-substituted tetra­zoles. Tetra­zolato (tz) ligands, with their four N-atom lone pairs, display a wide variety of coordination modes (Massi et al., 2018[Massi, M., Stagni, S. & Ogden, M. I. (2018). Coord. Chem. Rev. 375, 164-172.]; Aromí et al., 2011[Aromí, G., Barrios, L. A., Roubeau, O. & Gamez, P. (2011). Coord. Chem. Rev. 255, 485-546.]) from monodentate to polydentate, engaging multiple metal centers in coordination clusters or polymers. We were inter­ested in isolating discrete com­plexes of Ti, Zr, and Ta with a tz ligand that would display either 1,2-η2 or 2,3-η2 coordination, because such coordination by non­bridging tz ligands has not been reported for the d-block elements. The 1,2-η2 coordination by a nonbridging tz ligand has been reported for Ba (Kobrsi et al., 2005[Kobrsi, I., Knox, J. E., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2005). Inorg. Chem. 44, 4894-4896.]), Cs (Hernández-Arganis et al., 2018[Hernández-Arganis, M., Moya-Cabrera, M., Jancik, V., Martínez-Otero, D., María Cotero-Villegas, A., del Carmen Pérez-Redondo, M. & Cea-Olivares, R. (2018). Inorg. Chim. Acta, 475, 83-89.]), K (Kobrsi et al., 2006[Kobrsi, I., Zheng, W., Knox, J. E., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2006). Inorg. Chem. 45, 8700-8710.]; Zheng et al., 2003[Zheng, W., Heeg, M. J. & Winter, C. H. (2003). Angew. Chem. Int. Ed. 42, 2761-2764.]; Hu et al., 2005[Hu, X.-R., Wang, Y.-W. & Gu, J.-M. (2005). Acta Cryst. E61, m1686-m1688.]), Sm (Evans et al., 1988[Evans, W. J., Drummond, D. K., Hughes, L. A., Zhang, H. & Atwood, J. L. (1988). Polyhedron, 7, 1693-1703.]), and actinides U and Th (Browne et al., 2016[Browne, K. P., Maerzke, K. A., Travia, N. E., Morris, D. E., Scott, B. L., Henson, N. J., Yang, P., Kiplinger, J. L. & Veauthier, J. M. (2016). Inorg. Chem. 55, 4941-4950.]), whereas the 2,3-η2 coordination by a nonbridging tz ligand has only been reported for Ba (Kobrsi et al., 2005[Kobrsi, I., Knox, J. E., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2005). Inorg. Chem. 44, 4894-4896.]).

The multidentate nature of the 5-phenyl­tetra­zolato (Tz) ligand selected for these studies promotes dimerization; thus, all three com­plexes reported herein are dimeric, and only the Zr com­plex contains a desired 1,2-η2 coordination (Fig. 1[link]). To the best of our knowledge, this is the first structural report of a d-block element with a 1,2-η2 coordination of a nonbridging tz ligand. In all three com­plexes, Tz moieties are involved in hy­dro­gen-bonding inter­actions. Inter­estingly, the fate of the di­methyl­amido ligands present in the starting materials Ti(NMe2)4, Zr(NMe2)4, and Ta(NMe2)5 is different in the three synthetic reactions, as they are either retained or converted to either di­methyl­amine or di­methyl­ammonium. In the cases of Ti and Ta, the final products contain amido ligands and di­methyl­ammonium cations; in the Zr case, some groups remain amido, whereas some become coordinated di­methyl­amines. The di­methyl­amine is coordinated as a neutral ligand and di­methyl­ammonium is retained as a hy­dro­gen-bonded entity bridging Tz ligands. Numerous metal com­plexes with [Me2NHx]n, where x = 0, 1, or 2, and n = −1, 0, or +1, respectively, have been reported in the Cambridge Structural Database (CSD; Groom et al., 2016[Groom, C. R., Bruno, I. J., Lightfoot, M. P. & Ward, S. C. (2016). Acta Cryst. B72, 171-179.]).

[Figure 1]
Figure 1
The Ti, Zr, and Ta com­plexes (a) 1, (b) 2, and (c) 3, shown with their formulae.

Herein we report three related, but diverse, crystal structures of dinuclear com­plexes, namely, di­methyl­ammonium tris­(μ-5-phenyl­tetra­zolato-κ2N2:N3)bis­[bis­(di­methyl­amido)(5-phenyl­tetra­zolato-κN2)titanium(IV)] benzene 1.45-solvate, (Me2NH2)[Ti2(NMe2)4(2,3-μ-Tz)3(2-η1-Tz)2]·1.45C6H6, (1·1.45C6H6), bis­(di­methyl­amido)-1κN,2κN-bis­(di­methyl­amine)-1κN,2κN-tris­(μ-5-phenyl­tetra­zolato-1:2κ2N2:N3)tris­(5-phenyl­tetra­zolato)-1κ2N2;2κ2N2,N3-dizirconium(IV)]–benzene–di­chloro­methane (1/1.12/0.38), [Zr2(Me2NH)2(NMe2)2(2,3-μ-Tz)3(2-η1-Tz)2(1,2-η2-Tz)]·1.12C6H6·0.38CH2Cl2 (2·1.12C6H6·0.38CH2Cl2), and bis­(di­methyl­ammonium) μ-oxido-bis­(μ-5-phenyl­tetra­zolato-κ2N2:N3)bis­[(di­methyl­amido)­tris­(5-phenyl­tetra­zolato-κN2)tantalum(V)] toluene 0.25-solvate, (Me2NH2)2[Ta2(NMe2)2(2,3-μ-Tz)2(2-η1-Tz)6O]·0.25C7H8 (3·0.25C7H8). The Zr and Ta com­plexes crystallize with two symmetry-independent mol­ecules in the asymmetric unit; the second symmetry-independent mol­ecules are labelled in a similar fashion with `A' as the label suffix.

2. Experimental

2.1. Synthesis and crystallization

Complex 1 was prepared and crystallized according to a published procedure (Guzei, 1997[Guzei, I. A. (1997). PhD thesis, Wayne State University, MI, USA.]). Complexes 2 and 3 were prepared in a similar manner and crystallized from CH2Cl2/benzene and toluene, respectively. Adventitious oxygen became incorporated in Ta com­plex 3; no further attempts were made to repeat its synthesis.

2.2. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1[link]. The diffraction data collections were performed by standard techniques on Bruker area-detector single-crystal diffractometers at 100 K with APEX3 (Bruker, 2018[Bruker (2018). APEX3 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]), the data were scaled with SADABS (Krause et al., 2015[Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3-10.]), and the structures solved with SHELXS and SHELXT (Sheldrick, 2015a[Sheldrick, G. M. (2015a). Acta Cryst. A71, 3-8.]), and refined with SHELXL (Sheldrick, 2015b[Sheldrick, G. M. (2015b). Acta Cryst. C71, 3-8.]) and OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]).

Table 1
Experimental details

Experiments were carried out with Mo Kα radiation using a Bruker SMART APEX CCD area-detector diffractometer. Absorption was corrected for by multi-scan methods (SADABS; Krause et al., 2015[Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3-10.]).

  1 2 3
Crystal data
Chemical formula (C2H8N)[Ti2(C7H5N4)5(C2H6N)4]·1.45C6H6 [Zr2(C7H5N4)6(C2H6N)2(C2H7N)2]·1.118C6H6·0.382CH2Cl2 (C2H8N)2[Ta2(C7H5N4)8(C2H6N)2O]·0.25C7H8
Mr 1043.95 1351.41 1742.47
Crystal system, space group Monoclinic, P21/c Triclinic, P[\overline{1}] Monoclinic, P21/n
Temperature (K) 100 100 105
a, b, c (Å) 11.6292 (9), 22.6611 (17), 22.3631 (17) 13.9631 (5), 16.7619 (6), 27.3054 (9) 22.5131 (8), 25.5101 (9), 26.7165 (9)
α, β, γ (°) 90, 93.857 (1), 90 86.902 (1), 81.154 (1), 89.969 (1) 90, 101.3830 (4), 90
V3) 5880.0 (8) 6305.3 (4) 15041.8 (9)
Z 4 4 8
μ (mm−1) 0.32 0.43 2.98
Crystal size (mm) 0.4 × 0.3 × 0.2 0.4 × 0.3 × 0.2 0.39 × 0.32 × 0.24
 
Data collection
Tmin, Tmax 0.576, 0.745 0.578, 0.745 0.4, 0.5
No. of measured, independent and observed [I > 2σ(I)] reflections 46383, 11558, 8907 70012, 25682, 20488 173076, 29545, 25534
Rint 0.042 0.040 0.030
(sin θ/λ)max−1) 0.617 0.626 0.617
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.050, 0.142, 1.09 0.039, 0.103, 1.01 0.027, 0.068, 1.09
No. of reflections 11558 25682 29545
No. of parameters 826 1671 1915
No. of restraints 898 67 79
H-atom treatment H-atom parameters constrained H atoms treated by a mixture of independent and constrained refinement H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 0.53, −0.42 0.78, −0.98 2.48, −1.24
Computer programs: APEX3 (Bruker, 2018[Bruker (2018). APEX3 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]), SAINT (Bruker, 2018[Bruker (2018). APEX3 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]), SHELXS (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]), olex2.solve (Bourhis et al., 2015[Bourhis, L. J., Dolomanov, O. V., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2015). Acta Cryst. A71, 59-75.]), SHELXT (Sheldrick, 2015a[Sheldrick, G. M. (2015a). Acta Cryst. A71, 3-8.]), SHELXL2018 (Sheldrick, 2015b[Sheldrick, G. M. (2015b). Acta Cryst. C71, 3-8.]), SHELXL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]), and OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]).

Compound 1·1.45C6H6 crystallizes with a monoanionic dinuclear titanium com­plex, a di­methyl­ammonium cation, and ∼1.45 mol­ecules of benzene solvent in the asymmetric unit. The phenyl (Ph) rings at C12 and C26 are disordered over two positions, with major com­ponent contributions of 60.6 (13) and 77 (3)%, respectively. The Ph ring at C19 is disordered over three positions in a 43.4 (3):35.6 (3):21.0 (3) ratio. The disordered rings were refined with an idealized geometry and atomic displacement parameter restraints. The di­methyl­ammonium cation is disordered over two positions, with the major com­ponent present 54.3 (15)% of the time. The fully occupied solvent mol­ecule appeared to be benzene disordered over several positions. The other solvent mol­ecule was disordered over a crystallographic inversion center. A significant amount of time was invested in identifying and refining the disordered mol­ecules. Bond-length restraints were applied to model the mol­ecules but the resulting isotropic displacement coefficients suggested the mol­ecules were mobile. In addition, the refinement was com­putationally unstable. The SQUEEZE option (Spek, 2015[Spek, A. L. (2015). Acta Cryst. C71, 9-18.]) of PLATON (Spek, 2020[Spek, A. L. (2020). Acta Cryst. E76, 1-11.]) was used to correct the diffraction data for diffuse scattering effects and to identify the solvate mol­ecule. PLATON calculated the upper limit of volume that can be occupied by the solvent to be 910 Å3, or 15.5% of the unit-cell volume. The program calculated 246 electrons in the unit cell for the diffuse species. This approximately corresponds to one mol­ecule of benzene (42 e) and 0.45 mol­ecules of either benzene or CH2Cl2 (19 e) in the asymmetric unit. All derived results in the tables are based on the known contents. No data are given for the diffusely scattering species. This com­plex proved to be challenging to characterize and several data sets were collected on crystals isolated from several different syntheses.

Compound 2 crystallizes with two symmetry-independent dinuclear com­plexes in the asymmetric unit and several mol­ecules of crystallization solvents. The solvent mol­ecules occupy three different sites: (i) one fully occupied mol­ecule of benzene; (ii) a site shared by benzene and CH2Cl2 in a 64.3 (2):35.7 (2) ratio; (iii) a site shared by CH2Cl2/benzene­(orientation #1)/benzene­(orientation #2) in a 40.6 (2):35.7 (2):23.7 (2) ratio. The asymmetric unit content is 22.(benzene)2.24(CH2Cl2)0.76. The disordered benzene mol­ecules were refined with idealized geometries and atomic displacement parameter restraints. Atoms C19S–C24S of the 23.7%-occupied benzene mol­ecule were refined with identical isotropic atomic displacement parameters. The 40.6%-occupied di­chloro­methane mol­ecule was refined with geometrical restraints.

Compound 3 crystallizes with two symmetry-independent mol­ecules of the dinuclear dianioninc Ta com­plex, four di­methyl­ammonium cations, and half a mol­ecule of toluene solvent in the asymmetric unit. The toluene mol­ecule is disordered over a crystallographic inversion center and was refined with an idealized geometry (Guzei, 2014[Guzei, I. A. (2014). J. Appl. Cryst. 47, 806-809.]). The Ph ring at atom C52 is disordered over two positions, with the major com­ponent occupied 52 (2)% of the time. The disordered Ph rings were refined with an idealized geometry and atomic displacement parameter restraints.

3. Results and discussion

The three com­plexes reported herein exemplify the remarkable structural diversity of dinuclear com­plexes of metals from periods IV, V, and VI with Tz and di­methyl­amido ligands (Table 2[link]). These com­plexes possess different charges: the titanium com­plex is anionic, the tantalum com­plex dianionic, and the zirconium com­plex neutral. The charges are balanced by an appropriate number of di­methyl­ammonium cations that form N—H⋯N inter­actions with Tz ligands residing on different metal atoms. All metal centers bear di­methyl­amido ligands, but in addition the Zr centers bind to a neutral di­methyl­amine. Each metal is also ligated by two or three bridging μ-η1(N2):η1(N3) Tz ligands. The Ti, Zr, and Ta centers are further coordinated to terminal η1(N2) Tz ligands; inter­estingly, the titanium centers bear one such ligand, zirconium zero or two, and tantalum three. Strikingly, one Zr center does not bear terminal Tz ligands and instead features an η2(N1,N2) Tz moiety. The tantalum com­plex also contains a μ-oxo bridge, apparently due to a serendipitous incorporation of adventitious oxygen into the reaction mixture.

Table 2
Ligand com­position of com­plexes 13

  Compound
  1 2 3
Charge −1 0 0 −2
   
Ligand Metal center
  Ti Zr1 Zr2 Ta
NMe2 2 1 1 1
HNMe2 0 1 1 0
μ-Tz 3 3 3 2
η1-Tz terminal 1 2 0 3
η2-Tz terminal 0 0 1 0
μ-oxo 0 0 0 1
Number of hy­dro­gen-bonded Me2NH2+ 1 0 0 2

In the monoanionic dinuclear com­plex 1, the two six-coordinate Ti centers are separated by 4.2668 (6) Å (Fig. 2[link]). Each Ti atom is ligated by two NMe2 ligands, three μ-η1(N2):η1(N3) Tz ligands, and one terminal η1(N2) Tz moiety. The charge is balanced by a di­methyl­ammonium cation that forms a hy­dro­gen bond to each terminal Tz ligand. The four Ti—NMe2 distances (Table 3[link]) average 1.894 (5) Å and are in excellent agreement with the literature value of 1.91 (2) Å obtained by averaging 84 Ti—NMe2 bonds observed in 44 com­plexes reported in the CSD. The Ti—N(terminal Tz) bond lengths in 1 are very similar and expectedly longer at an average of 2.152 (2) Å. There is only one Ti com­plex with a monodentate η1(N2)-Tz ligand reported to the CSD, i.e. tris­(3,5-di-tert-butyl­pyrazolato)(5-phenyl­tetra­zolato)titanium(IV) (Yélamos et al., 2001[Yélamos, C., Gust, K. R., Baboul, A. G., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2001). Inorg. Chem. 40, 6451-6462.]), and one with a neutral η1(N2)-TzH ligand, [TiCl4(PhCN4H)2] (Hill et al., 2004[Hill, M. S., Hitchcock, P. B. & Smith, N. (2004). Polyhedron, 23, 801-807.]). The Ti—N(Tz) and Ti—N(TzH) distances in these were determined to be 2.104 Å (low precision room-tem­per­a­ture data set), with an average of 2.272 (7) Å. Predictably, the Ti—N(bridging Tz) bonds in 1 are even longer, and fall into two groups because the com­position of the outer coordination sphere differs among the three bridging Tz ligands. Complex 1 may be described as pseudo-C2v-symmetrical, with one mirror plane roughly containing both terminal and one bridging Tz ligands. The Ti—N bond distances to the bridging N8-tetra­zolato ligand in the mirror plane are shorter [average 2.1970 (19) Å] than the other four Ti—N bridging distances [average 2.26 (2) Å], and the difference is statistically significant. This disparity can be explained by the relative location of these ligands. Atoms N8 and N9 of the bridging ligand in the mirror plane are trans to tz rings, whereas the ligated N atoms in the other bridging ligands are trans to π-electron-donating NMe2 units. The charge-assisted hy­dro­gen bonds between the [H2NMe2]+ cation and the Tz ligands are asymmetrical, with DA and D—H⋯A parameters of 2.690 (8)/160 and 2.847 (8) Å/154° for one position of the disordered cation, and 2.742 (7)/156 and 2.864 (8) Å/169° for the other (Table 4[link]).

Table 3
Selected bond lengths (Å) for 1

Ti1—N3 2.1534 (19) Ti2—N9 2.1970 (19)
Ti1—N5 1.892 (2) Ti2—N13 2.2404 (19)
Ti1—N6 1.893 (2) Ti2—N17 2.266 (2)
Ti1—N8 2.1967 (18) Ti2—N19 1.901 (2)
Ti1—N12 2.2592 (19) Ti2—N20 1.890 (2)
Ti1—N16 2.294 (2) Ti2—N23 2.151 (2)

Table 4
Hydrogen-bond geometry (Å, °) for 1

D—H⋯A D—H H⋯A DA D—H⋯A
N25—H25C⋯N22 0.91 1.89 2.742 (7) 156
N25—H25D⋯N2 0.91 1.97 2.864 (8) 169
N25A—H25E⋯N22 0.91 2.00 2.847 (8) 154
N25A—H25F⋯N2 0.91 1.82 2.690 (8) 160
[Figure 2]
Figure 2
A mol­ecular drawing of 1, shown with 30% probability displacement ellipsoids. Minor disorder com­ponents and H atoms not participating in hy­dro­gen bonds have been omitted.

The dinuclear Zr com­plex 2 (Fig. 3[link]) crystallizes with two sym­metry-independent com­plexes designated hereafter 2a, with atoms Zr1 and Zr2, and 2b, with atoms Zr1A and Zr2A in the asymmetric unit. Complexes 2a and 2b are the only neutral ones in this series. They possess identical com­positions, but a superposition of the two mol­ecules clearly illustrates their conformational differences (Fig. 4[link]). In the following discussion we will focus on Zr1 com­plex 2a and provide data for 2b as necessary. The two Zr atoms in 2a are seven-coordinate, but have different coordination environments: Zr1 is ligated by a NMe2, HNMe2, three bridging μ-η1(N2):η1(N3) Tz ligands, and two terminal η1(N2) Tz ligands; Zr2 is ligated similarly, except that the two terminal Tz ligands are replaced by one bidentate η2(N1,N2) Tz fragment. The Zr⋯Zr separations in 2a and 2b are 4.5230 (3) and 4.5492 (3) Å, respectively, the latter being ∼0.27 Å longer than the Ti⋯Ti distance in 1.

[Figure 3]
Figure 3
A mol­ecular drawing of 2a, shown with 30% probability displacement ellipsoids. All H atoms not participating in hy­dro­gen bonds have been omitted.
[Figure 4]
Figure 4
Superposition of 2a and 2b. All H atoms have been omitted. Complex 2b is shown in monochrome.

The η2(N1,N2) ligation mode of a nonbridging tz ring in Zr com­plex 2 is particularly exciting because it is the first structural report of a d-block element with this coordination mode. Based on a CSD search, such a coordination has been re­por­ted only for metals with atomic radii ≥ 1.75 Å (Slater, 1964[Slater, J. C. (1964). J. Chem. Phys. 41, 3199-3204.]), i.e. Ba with 5-(di­methyl­amino)tz (Kobrsi et al., 2005[Kobrsi, I., Knox, J. E., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2005). Inorg. Chem. 44, 4894-4896.]), Cs with (1-phenyl-5-thione)tz (Hernández-Arganis et al., 2018[Hernández-Arganis, M., Moya-Cabrera, M., Jancik, V., Martínez-Otero, D., María Cotero-Villegas, A., del Carmen Pérez-Redondo, M. & Cea-Olivares, R. (2018). Inorg. Chim. Acta, 475, 83-89.]), K with 5-(pyrrolidin-1-yl)tz, 5-tButz (Kobrsi et al., 2006[Kobrsi, I., Zheng, W., Knox, J. E., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2006). Inorg. Chem. 45, 8700-8710.]), Tz (Zheng et al., 2003[Zheng, W., Heeg, M. J. & Winter, C. H. (2003). Angew. Chem. Int. Ed. 42, 2761-2764.]), and losartanide (Hu et al., 2005[Hu, X.-R., Wang, Y.-W. & Gu, J.-M. (2005). Acta Cryst. E61, m1686-m1688.]), Sm with 1,5-penta­methyl­ene-tetra­zole (Evans et al., 1988[Evans, W. J., Drummond, D. K., Hughes, L. A., Zhang, H. & Atwood, J. L. (1988). Polyhedron, 7, 1693-1703.]), and actinides U and Th with 5-Metz (Browne et al., 2016[Browne, K. P., Maerzke, K. A., Travia, N. E., Morris, D. E., Scott, B. L., Henson, N. J., Yang, P., Kiplinger, J. L. & Veauthier, J. M. (2016). Inorg. Chem. 55, 4941-4950.]). A bridging μ-η1(N3):η2(N1,N2) tz ring has been observed in dimeric com­plexes of Dy, Gd, Ho, Y, and Yb, and polydentate η2(N1,N2) tetra­zolato ligands have been reported for the alkali metals Na, K, Cs, and Rb. The only example with an η2(N2,N3) tz ligand has been reported for another large-atomic-radius-atom Ba (Kobrsi et al., 2005[Kobrsi, I., Knox, J. E., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2005). Inorg. Chem. 44, 4894-4896.]). The atomic radius of Zr (1.55 Å) is noticeably smaller than the atomic radii of the elements listed above, but larger than those of Ti (1.40 Å) or Ta (1.45 Å), thus a large soft metal center is not a prerequisite for the formation of an η2-tetra­zolato com­plex.

In order to better understand the bidentate coordination mode of the tetra­zolato ligand, a series of density functional theory (DFT) minimizations were performed on a model com­plex Zr(Tz)Cl3 at the B3LYP/SDD level of theory. In these com­plexes, with largely ionic metal–ligand bonding, the com­plex with the 2,3-η2 ligand is 0.34 kcal mol−1 more stable than the 1,2-η2 analogue. Similar results were reported for model com­plexes tri­chloro­[(1,2-η)-5-methyl­tetra­zolato]titanium(IV) and tri­chloro­[(2,3-η)-5-methyl­tetra­zolato]titanium(IV), with the latter being more stable by less than 0.8 kcal mol−1 (Yélamos et al., 2001[Yélamos, C., Gust, K. R., Baboul, A. G., Heeg, M. J., Schlegel, H. B. & Winter, C. H. (2001). Inorg. Chem. 40, 6451-6462.]). This is in slight contrast to the expectation based on the natural atomic charges com­puted for a free Tz anion: this analysis indicated that the N atoms in the 1- and 4-positions are more nucleophilic (by −0.21) than the 2- and 3-position N atoms, which means that a pair of adjacent atoms 1 and 2 (or 3 and 4) carries a larger combined negative charge than a combination of atoms 2 and 3, and that should favour the 1,2-η2 binding mode.

Steric considerations may play a decisive role when several ligand arrangements are similar in energy. The different coordination environments of the metal centers in 2 deserve a special scrutiny with the use of G-parameters that are based on ligand solid angles (Guzei & Wendt, 2006[Guzei, I. A. & Wendt, M. (2006). Dalton Trans. pp. 3991-3999.]). The G-parameter describes ligand steric effects and represents the per­cen­tage of the metal coordination sphere shielded by a given ligand. In the model com­plex Zr(1,2-η2-Tz)Cl3 (Fig. 5[link]), the bidentate ligand shields the metal to the extent of 21.0 (2)%, and in Zr(2,3-η2-Tz)Cl3, the corresponding parameter is 20.2 (2)%. The small difference between these values is not as counterintuitive as it may seem based on the position of the Ph ring, because the metal centers are primarily shielded by the ligated N atoms. The coordination environment of the metals in these model com­plexes is not crowded because the four ligands shield no more than 62% of the metal; thus, sterics is unlikely to explain the com­putational results. Either bidentate coordination mode of Tz is viable for zirconium and the rationale for the observed 1,2-η2 coordination may be found in the crystal packing forces.

[Figure 5]
Figure 5
Model zirconium(IV) com­plexes used to evaluate the stability of the two coordination modes of the Tz ligand. The numbers are the G-parameters for the Tz ligands. The bottom figures illustrate how the bidentate ligands shield the metal – the colored portions of the sphere are ligands' `shadows' on a 12 Å sphere they would cast if the metal were replaced with a light source. The view is from the position of the Tz ligand down toward the metal. The shadow is blue for the Tz ligand, and red, fuchsia, and turquoise for the Cl atoms.

Steric considerations become more com­plicated for experimentally observed geometries because the G-parameters may change depending on ligand conformations and orientations relative to the metal center. G-Parameters become smaller with increasing metal–ligand distances. Overall, atom Zr1 is shielded by seven ligands to an extent of 85% and atom Zr2 is shielded similarly up to 84% by six ligands. The G-parameters for the two terminal η1-Tz ligands on atom Zr1 add up to 22%, whereas the sole η2-Tz ligand on Zr2 shields 18% of the zirconium coordination sphere.

We note that the bond distances between the three bridging Tz ligands and Zr1 are slightly longer than those to Zr2; these ligands approach Zr2 closer and shield it by an additional 1% each. Consequently, the overall difference in the Zr1 and Zr2 G-parameters is only 1% (85 versus 84%).

Whereas the Zr—NMe2 distances to each metal center are similar (Table 5[link]), the Zr—NHMe2 bond lengths are statistically significantly different. This distance to the seven-ligand-bearing Zr1 center is longer at 2.4073 (19) Å than to the six-ligand-ligated Zr2 atom at 2.3218 (19) Å. Both distances fall in the 2.308–2.574 Å range observed for Zr—NHMe2 distances com­puted for 50 such bonds in 37 com­plexes reported to the CSD. The HNMe2 ligands occupy different positions in the coordination spheres of each metal, as can be readily illustrated by the Zr⋯Zr—NHMe2 angles. The Zr1⋯Zr2—NHMe2 and Zr2⋯Zr1—NHMe2 angles span the range 107.65 (5)–145.45 (5)°. The di­methyl­amine ligands participate in intra­molecular hy­dro­gen-bonding inter­actions (Table 6[link]). The HNMe2 ligand on the seven-ligand-bearing Zr1 center forms an N—H⋯N hy­dro­gen bond to a terminal Tz ligand, whereas the HNMe2 ligand on the six-ligand-ligated Zr2 atom forms a hy­dro­gen bond to a bridging tz ring.

Table 5
Selected bond lengths (Å) for 2

Zr1—N2 2.2935 (18) Zr1A—N2A 2.2856 (19)
Zr1—N6 2.3340 (19) Zr1A—N6A 2.3073 (19)
Zr1—N9 1.9798 (19) Zr1A—N9A 1.987 (2)
Zr1—N10 2.4073 (19) Zr1A—N10A 2.4095 (19)
Zr1—N12 2.3829 (18) Zr1A—N12A 2.3907 (18)
Zr1—N16 2.3741 (18) Zr1A—N16A 2.3651 (19)
Zr1—N20 2.3699 (19) Zr1A—N20A 2.3822 (19)
Zr2—N13 2.3115 (19) Zr2A—N13A 2.2969 (18)
Zr2—N17 2.3085 (17) Zr2A—N17A 2.336 (2)
Zr2—N21 2.3227 (18) Zr2A—N21A 2.3166 (19)
Zr2—N23 2.3027 (19) Zr2A—N23A 2.290 (2)
Zr2—N24 2.2238 (19) Zr2A—N24A 2.214 (2)
Zr2—N27 2.3218 (19) Zr2A—N27A 2.3145 (19)
Zr2—N28 1.975 (2) Zr2A—N28A 1.989 (2)

Table 6
Hydrogen-bond geometry (Å, °) for 2

D—H⋯A D—H H⋯A DA D—H⋯A
N10—H10⋯N5 0.85 (2) 1.96 (2) 2.732 (3) 151 (2)
N27—H27⋯N22 0.84 (2) 2.35 (2) 2.965 (3) 130 (2)
N10A—H10B⋯N5A 0.85 (2) 2.16 (2) 2.902 (3) 145 (2)
N27A—H27A⋯N22A 0.85 (2) 2.33 (2) 2.940 (3) 129 (2)

The Zr—N(bridging) distances to Zr1 and Zr2 are dissimilar, and the difference is statistically significant. These bond distances to the seven-ligand-bearing Zr1 center [average 2.376 (7) Å] are longer than the respective bonds to Zr2 [average 2.314 (7) Å], a behaviour also observed for the di­methyl­amine ligands. Bond distances are expected to be longer for metals with higher coordination numbers, but, in this case, the formal coordination number is the same and the two metals differ only in the number of ligands.

The Zr1—N(terminal Tz) distances are expectedly longer than Zr2—N(bidentate Tz). The coordination mode of the η2(N1,N2)Tz may be described as `slipped', with the Zr2—N23 distance to the N atom closest to the Ph ring being noticeably longer [2.3027 (19) Å] than the Zr2—N24 bond to the N atom in the second ring position [2.2238 (19) Å]. The difference can be rationalized in terms of the steric requirement of the Ph ring that does not allow a closer approach of N23 to Zr2.

The structure of 3·0.5C7H8 appears to be the first example of a structurally characterized Ta com­plex bearing a tz ligand. In the structure, there are two symmetry-independent dinuclear Ta com­plexes (3a and 3b), with an identical com­position and very similar geometries about the metal centers (Fig. 6[link]). The com­plexes differ mainly in the positions and conformations of the Tz ligands (Fig. 7[link]). Each Ta center is seven-coordinated, with the coordination sphere com­prised of an NMe2 ligand, two bridging and three η2(N2)-terminal Tz ligands, and a bridging oxo ligand (Table 7[link]). The two bridging Tz ligand rings connect the Ta centers in the same μ-η1(N2):η1(N3) arrangement observed for corresponding ligands in 1 and 2. The Ta⋯Ta separation averages 3.645 (2) Å for the two com­plexes, and is the shortest metal–metal distance in this series by a large margin, undoubtedly due to the presence of the oxo bridge. The metal–ligand bond distances fall into three well-separated ranges: the Ta—NMe2 and Ta—O bond lengths are similar at ∼1.93 Å, the Ta—N(terminal Tz) are longer at ∼2.21 Å, and Ta—N(bridging Tz) are the longest at ∼2.27 Å. The com­plex exhibits a very approximate C2v symmetry, with atoms Ta1, O1, and Ta2 defining one of the mirror planes. The dihedral angles between the tz-ring planes of the bridging ligands are 78.53 (10) and 75.43 (10)° in 3a and 3b, respectively, which is substanti­ally smaller than the ideal 120° angle that could be expected between three bridging ligands.

Table 7
Selected bond lengths (Å) for 3

Ta1—O1 1.938 (2) Ta1A—O1A 1.932 (2)
Ta1—N2 2.204 (3) Ta1A—N2A 2.204 (3)
Ta1—N6 2.202 (3) Ta1A—N6A 2.210 (3)
Ta1—N10 2.213 (3) Ta1A—N10A 2.211 (3)
Ta1—N13 1.924 (3) Ta1A—N13A 1.929 (3)
Ta1—N15 2.265 (3) Ta1A—N19A 2.280 (3)
Ta1—N19 2.283 (3) Ta1A—N15A 2.249 (3)
Ta2—O1 1.921 (2) Ta2A—O1A 1.932 (2)
Ta2—N16 2.280 (3) Ta2A—N20A 2.269 (3)
Ta2—N20 2.281 (3) Ta2A—N16A 2.273 (3)
Ta2—N23 2.204 (3) Ta2A—N23A 2.217 (3)
Ta2—N27 2.218 (3) Ta2A—N27A 2.215 (3)
Ta2—N31 2.194 (3) Ta2A—N31A 2.211 (3)
Ta2—N34 1.928 (3) Ta2A—N34A 1.928 (3)
[Figure 6]
Figure 6
(a) A mol­ecular drawing of 3a, shown with 40% probability displacement ellipsoids. All H atoms and minor disorder com­ponents have been omitted. (b) Hydrogen-bonding inter­actions between two H2NMe2 cations and dianionic Ta com­plex 3a.
[Figure 7]
Figure 7
Superposition of 3a and 3b. All H atoms and minor disorder com­ponents have been omitted. Complex 3b is shown in monochrome.

Two di­methyl­ammonium cations com­plete the second coordination sphere of each com­plex in a notable fashion by forming a total of six charge-assisted hy­dro­gen-bonding inter­actions. One [H2NMe2]+ forms one hy­dro­gen bond to a terminal Tz ligand on one Ta atom, and a bifurcated N—H⋯N(Tz) hy­dro­gen bond with its second acidic proton to two Tz ligands from the other Ta center (Table 8[link]). These three hy­dro­gen-bonding inter­actions involve three of the six terminal Tz moieties. The other [H2NMe2]+ cation forms similar inter­actions with the three remaining Tz ligands, but the connectivity of the single and bifurcated hy­dro­gen bonds is reversed relative to the Ta centers. The single N—H⋯N hy­dro­gen bonds average 2.85 (2) Å, with the D—H⋯A angles in the range 149–161°. The bifurcated bonds are appreciably longer, with an average of 2.99 (5) Å, and their suboptimal D—H⋯A angles span the range 121–150°. Whereas there are no Ta–tz com­plexes and no closely related seven-coordinated Ta com­plexes with Ta—O—Ta bridges reported to the CSD, there are 164 com­plexes with a Ta—NMe2 fragment. In these, the Ta—N distances in the four-, five-, six-, seven-, eight-, and nine-coordinate com­plexes averaged 1.98 (3), 1.98 (3), 2.00 (5), 2.01 (3), 1.970 (15), and 1.990 (6) Å, respectively. The differences among these values are not statistically significant, and the expected trend of metal–ligand distance elongation with the increase in the metal coordination number is absent. The Ta—NMe2 distances in 3a and 3b are much shorter at 1.93 Å, and are among the shortest bond lengths of this type reported to the CSD. This is probably a result of the dianionic nature of the com­plexes.

Table 8
Hydrogen-bond geometry (Å, °) for 3

D—H⋯A D—H H⋯A DA D—H⋯A
N35—H35B⋯N24 0.91 2.00 2.875 (4) 161
N35—H35C⋯N3 0.91 2.46 3.031 (4) 121
N35—H35C⋯N7 0.91 2.12 2.943 (4) 150
N36—H36B⋯N11 0.91 1.98 2.836 (4) 156
N36—H36C⋯N28 0.91 2.17 2.978 (5) 148
N36—H36C⋯N32 0.91 2.44 3.085 (4) 128
N35A—H35D⋯N3A 0.91 2.05 2.867 (4) 149
N35A—H35E⋯N24A 0.91 2.33 2.994 (4) 130
N35A—H35E⋯N28A 0.91 2.20 2.954 (4) 140
N36A—H36D⋯N7A 0.91 2.23 2.961 (4) 137
N36A—H36D⋯N11A 0.91 2.34 2.981 (4) 127
N36A—H36E⋯N32A 0.91 1.95 2.828 (4) 161

4. Conclusions

This work expands the number of structurally characterized com­plexes of Ti, Zr, and Ta with tetra­zolato ligands. All three com­plexes are dinuclear; the Ti center in 1 is six-coordinate, whereas the Zr and Ta atoms in 2 and 3 are seven-coordinate. The coordination environments of the Ti centers 1 and Ta centers in 3 are similar; however, the two Zr centers in 2 bear a different number of ligands, one of which is a bidentate 1,2-η2-Tz ligand, not previously observed for d-block elements. The starting materials for the chemical reactions leading to the isolation of 13 involved di­methyl­amido ligands that were (a) retained in the products, (b) converted to di­methyl­amine eliminated from the reaction mixture by gas evolution, (c) converted to di­methyl­amine and retained as a neutral ligand, and (d) converted to di­methyl­ammonium and retained as a hy­dro­gen-bonded entity bridging Tz ligands. These relatively large metal com­plexes crystallize with solvent-accessible voids in their lattices that are indeed occupied by ordered and disordered solvent mol­ecules. The refinement of the disordered solvent mol­ecules pre­sent­ed certain challenges but was accom­plished by standard techniques.

Supporting information


Computing details top

Bis(dimethylammonium) tris(µ-5-phenyltetrazolato-κ2N2:N3)bis[bis(dimethylamido)(5-phenyltetrazolato-κN2)titanium] benzene 1.45-solvate (1) top
Crystal data top
(C2H8N)[Ti2(C7H5N4)5(C2H6N)4]·1.45C6H6F(000) = 2184
Mr = 1043.95Dx = 1.179 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 11.6292 (9) ÅCell parameters from 22219 reflections
b = 22.6611 (17) Åθ = 2.2–26.4°
c = 22.3631 (17) ŵ = 0.32 mm1
β = 93.857 (1)°T = 100 K
V = 5880.0 (8) Å3Block, brown
Z = 40.4 × 0.3 × 0.2 mm
Data collection top
Bruker SMART APEX CCD area detector
diffractometer
11558 independent reflections
Radiation source: sealed tube8907 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 8 pixels mm-1θmax = 26.0°, θmin = 1.8°
ω and φ scansh = 1414
Absorption correction: multi-scan
(SADABS; Bruker, 2018)
k = 2727
Tmin = 0.576, Tmax = 0.745l = 2727
46383 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.050H-atom parameters constrained
wR(F2) = 0.142 w = 1/[σ2(Fo2) + (0.0726P)2 + 2.6632P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.001
11558 reflectionsΔρmax = 0.53 e Å3
826 parametersΔρmin = 0.41 e Å3
898 restraints
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ti10.74516 (3)0.20237 (2)0.62569 (2)0.02525 (11)
Ti20.56820 (4)0.29739 (2)0.75626 (2)0.02952 (12)
N10.76100 (19)0.02299 (8)0.68243 (9)0.0363 (5)
N20.73530 (18)0.08001 (9)0.68754 (9)0.0362 (5)
N30.76913 (16)0.10915 (8)0.64050 (9)0.0294 (4)
N40.81803 (16)0.07150 (8)0.60321 (9)0.0299 (4)
N50.89897 (17)0.22772 (9)0.61966 (9)0.0349 (5)
N60.70669 (17)0.18977 (8)0.54308 (9)0.0307 (4)
N70.71383 (17)0.33132 (8)0.58545 (8)0.0298 (4)
N80.68922 (16)0.29481 (8)0.62947 (8)0.0280 (4)
N90.63051 (16)0.32360 (8)0.66955 (8)0.0284 (4)
N100.61479 (17)0.37954 (8)0.65171 (9)0.0327 (4)
N110.50202 (16)0.14395 (8)0.63901 (9)0.0303 (4)
N120.56788 (16)0.18867 (8)0.65889 (8)0.0269 (4)
N130.51682 (16)0.21748 (8)0.70183 (8)0.0279 (4)
N140.41627 (18)0.19155 (9)0.71021 (10)0.0370 (5)
N150.88137 (18)0.18841 (9)0.75326 (9)0.0349 (5)
N160.78387 (17)0.21064 (8)0.72730 (9)0.0305 (4)
N170.72863 (18)0.24070 (9)0.76779 (9)0.0365 (5)
N180.7888 (2)0.23883 (10)0.82038 (10)0.0482 (6)
N190.42108 (19)0.33433 (9)0.74992 (9)0.0382 (5)
N200.6561 (2)0.35954 (9)0.79243 (10)0.0448 (5)
N210.5049 (2)0.18095 (9)0.89978 (9)0.0456 (6)
N220.5435 (3)0.19430 (9)0.84678 (10)0.0521 (7)
N230.52220 (19)0.25073 (9)0.83493 (9)0.0360 (5)
N240.46968 (17)0.27568 (8)0.88041 (9)0.0312 (4)
N250.6039 (10)0.0924 (3)0.7906 (3)0.0421 (19)0.543 (15)
H25C0.5821940.1300800.7982670.051*0.543 (15)
H25D0.6410100.0926790.7561070.051*0.543 (15)
C440.6849 (11)0.0717 (3)0.8404 (4)0.069 (3)0.543 (15)
H44A0.6497150.0772160.8786530.104*0.543 (15)
H44B0.7564900.0945170.8406200.104*0.543 (15)
H44C0.7018100.0297960.8348520.104*0.543 (15)
C450.5001 (11)0.0553 (4)0.7821 (4)0.064 (2)0.543 (15)
H45A0.5227440.0136780.7809460.096*0.543 (15)
H45B0.4577050.0658600.7442280.096*0.543 (15)
H45C0.4507830.0616730.8153310.096*0.543 (15)
N25A0.6630 (10)0.0979 (4)0.7979 (4)0.035 (2)0.457 (15)
H25E0.6445910.1347920.8101560.042*0.457 (15)
H25F0.6808360.1005820.7589600.042*0.457 (15)
C44A0.7669 (10)0.0776 (3)0.8344 (3)0.047 (2)0.457 (15)
H44D0.7586150.0871080.8766580.071*0.457 (15)
H44E0.8352480.0974900.8207770.071*0.457 (15)
H44F0.7753750.0348420.8299110.071*0.457 (15)
C45A0.5606 (11)0.0599 (4)0.8007 (5)0.047 (3)0.457 (15)
H45D0.5780490.0203760.7859150.070*0.457 (15)
H45E0.4963470.0768240.7758240.070*0.457 (15)
H45F0.5394540.0571140.8423080.070*0.457 (15)
C10.81178 (19)0.01926 (10)0.63002 (11)0.0289 (5)
C20.8566 (2)0.03605 (10)0.60636 (12)0.0342 (5)
C30.8650 (2)0.08629 (10)0.64193 (13)0.0417 (6)
H30.8386450.0851320.6812180.050*
C40.9111 (2)0.13801 (11)0.62100 (14)0.0462 (7)
H40.9160660.1720970.6457630.055*
C50.9495 (3)0.13989 (12)0.56437 (15)0.0527 (8)
H50.9810030.1753310.5497080.063*
C60.9423 (3)0.08998 (13)0.52871 (16)0.0676 (10)
H60.9700930.0910860.4897390.081*
C70.8947 (3)0.03829 (12)0.54941 (14)0.0541 (8)
H70.8885270.0044600.5243140.065*
C80.9758 (2)0.19549 (12)0.58311 (14)0.0471 (7)
H8A1.0097430.2226920.5551240.071*
H8B0.9324760.1647440.5605390.071*
H8C1.0373050.1772380.6089560.071*
C90.9601 (2)0.27473 (13)0.65306 (14)0.0482 (7)
H9A1.0192990.2574840.6810730.072*
H9B0.9055050.2973570.6754610.072*
H9C0.9967150.3009260.6250940.072*
C100.6296 (2)0.14369 (11)0.51734 (11)0.0366 (6)
H10A0.5721470.1615360.4888010.055*
H10B0.5905550.1242430.5494590.055*
H10C0.6747420.1145190.4965820.055*
C110.7545 (2)0.22302 (12)0.49464 (12)0.0418 (6)
H11A0.7941900.1959420.4687450.063*
H11B0.8094320.2523370.5116190.063*
H11C0.6921310.2430890.4710580.063*
C120.6664 (2)0.38283 (9)0.60019 (10)0.0290 (5)
C130.6743 (4)0.43560 (18)0.56075 (18)0.0289 (16)0.606 (13)
C140.7432 (6)0.43690 (13)0.51233 (19)0.0395 (15)0.606 (13)
H140.7856600.4028540.5024250.047*0.606 (13)
C150.7500 (8)0.48802 (15)0.47840 (17)0.0445 (17)0.606 (13)
H150.7971290.4889100.4453020.053*0.606 (13)
C160.6880 (6)0.53784 (15)0.4929 (2)0.0502 (19)0.606 (13)
H160.6926140.5727730.4696930.060*0.606 (13)
C170.6191 (4)0.53653 (19)0.5413 (3)0.0513 (19)0.606 (13)
H170.5766300.5705800.5512080.062*0.606 (13)
C180.6122 (4)0.4854 (2)0.5752 (3)0.0417 (17)0.606 (13)
H180.5651600.4845240.6083320.050*0.606 (13)
C13A0.6623 (6)0.4392 (2)0.5691 (3)0.032 (3)0.394 (13)
C14A0.6798 (10)0.43762 (18)0.5082 (3)0.039 (2)0.394 (13)
H14A0.6955180.4011560.4894300.047*0.394 (13)
C15A0.6744 (12)0.4894 (2)0.4748 (2)0.044 (3)0.394 (13)
H15A0.6863520.4883340.4332320.053*0.394 (13)
C16A0.6515 (8)0.54275 (19)0.5023 (3)0.043 (2)0.394 (13)
H16A0.6477320.5781390.4794840.051*0.394 (13)
C17A0.6340 (8)0.5443 (2)0.5632 (4)0.049 (3)0.394 (13)
H17A0.6182790.5807660.5819340.059*0.394 (13)
C18A0.6394 (9)0.4925 (3)0.5965 (3)0.036 (2)0.394 (13)
H18A0.6274460.4935890.6381330.043*0.394 (13)
C190.4092 (2)0.14691 (10)0.67089 (11)0.0342 (5)
C200.3063 (9)0.1090 (6)0.6666 (7)0.043 (3)0.434 (3)
C210.3064 (7)0.0584 (6)0.6315 (6)0.045 (3)0.434 (3)
H210.3726890.0483890.6110010.054*0.434 (3)
C220.2094 (9)0.0224 (4)0.6262 (5)0.055 (3)0.434 (3)
H220.2094410.0121660.6022070.066*0.434 (3)
C230.1124 (7)0.0370 (4)0.6562 (5)0.059 (3)0.434 (3)
H230.0461190.0124390.6525890.071*0.434 (3)
C240.1124 (9)0.0876 (5)0.6913 (6)0.071 (3)0.434 (3)
H240.0460440.0975980.7117650.085*0.434 (3)
C250.2093 (12)0.1236 (5)0.6965 (8)0.063 (3)0.434 (3)
H250.2092920.1581530.7205590.076*0.434 (3)
C20A0.3103 (11)0.1074 (7)0.6553 (7)0.038 (3)0.356 (3)
C21A0.3177 (8)0.0635 (7)0.6123 (6)0.039 (3)0.356 (3)
H21A0.3838660.0609550.5897990.047*0.356 (3)
C22A0.2282 (10)0.0233 (5)0.6024 (5)0.051 (3)0.356 (3)
H22A0.2332310.0067530.5729920.062*0.356 (3)
C23A0.1313 (8)0.0269 (5)0.6354 (5)0.061 (4)0.356 (3)
H23A0.0701650.0005500.6285350.073*0.356 (3)
C24A0.1239 (9)0.0708 (6)0.6783 (6)0.067 (3)0.356 (3)
H24A0.0577320.0733600.7008860.080*0.356 (3)
C25A0.2134 (12)0.1111 (6)0.6883 (7)0.052 (3)0.356 (3)
H25A0.2083670.1410680.7176950.063*0.356 (3)
C20B0.3157 (11)0.1033 (7)0.6750 (8)0.039 (4)0.210 (3)
C21B0.2851 (15)0.0673 (9)0.6261 (8)0.045 (4)0.210 (3)
H21B0.3295540.0678730.5919690.053*0.210 (3)
C22B0.1895 (15)0.0307 (8)0.6271 (8)0.054 (4)0.210 (3)
H22B0.1685510.0061160.5937190.065*0.210 (3)
C23B0.1245 (11)0.0299 (7)0.6771 (8)0.074 (5)0.210 (3)
H23B0.0591060.0048190.6777680.089*0.210 (3)
C24B0.1551 (11)0.0658 (7)0.7259 (7)0.083 (5)0.210 (3)
H24B0.1106630.0652780.7600690.099*0.210 (3)
C25B0.2507 (11)0.1025 (6)0.7249 (7)0.067 (4)0.210 (3)
H25B0.2716650.1270350.7583210.080*0.210 (3)
C260.8816 (2)0.20654 (11)0.81012 (11)0.0399 (6)
C270.9669 (6)0.1895 (3)0.8593 (2)0.0351 (15)0.77 (3)
C281.0814 (5)0.1834 (3)0.8460 (3)0.0444 (13)0.77 (3)
H281.1021690.1876300.8058880.053*0.77 (3)
C291.1654 (5)0.1711 (3)0.8915 (4)0.0532 (16)0.77 (3)
H291.2436680.1669520.8823910.064*0.77 (3)
C301.1350 (6)0.1649 (2)0.9502 (3)0.0491 (16)0.77 (3)
H301.1924960.1565460.9812620.059*0.77 (3)
C311.0206 (7)0.1710 (4)0.9635 (2)0.0515 (17)0.77 (3)
H310.9998240.1668181.0036300.062*0.77 (3)
C320.9365 (7)0.1833 (4)0.9180 (2)0.0440 (17)0.77 (3)
H320.8583230.1874960.9271280.053*0.77 (3)
C27A0.9879 (11)0.1984 (9)0.8493 (7)0.025 (3)0.23 (3)
C28A1.0937 (12)0.1801 (11)0.8305 (9)0.047 (4)0.23 (3)
H28A1.1061650.1787820.7889820.056*0.23 (3)
C29A1.1814 (11)0.1636 (10)0.8725 (12)0.051 (4)0.23 (3)
H29A1.2536930.1510880.8597340.061*0.23 (3)
C30A1.1632 (16)0.1655 (7)0.9333 (11)0.044 (4)0.23 (3)
H30A1.2230470.1542120.9620350.053*0.23 (3)
C31A1.057 (2)0.1838 (7)0.9521 (8)0.043 (4)0.23 (3)
H31A1.0448710.1850310.9935840.051*0.23 (3)
C32A0.9697 (17)0.2002 (7)0.9100 (7)0.032 (3)0.23 (3)
H32A0.8973410.2127260.9228320.039*0.23 (3)
C330.3098 (2)0.30692 (12)0.75896 (13)0.0452 (7)
H33A0.2772150.3244160.7941460.068*
H33B0.3204830.2644260.7653000.068*
H33C0.2572330.3135420.7235030.068*
C340.4053 (3)0.39726 (12)0.73812 (15)0.0553 (8)
H34A0.3689440.4157000.7717190.083*
H34B0.3558790.4026490.7012610.083*
H34C0.4803700.4156950.7334420.083*
C350.6108 (3)0.39493 (13)0.84034 (13)0.0600 (9)
H35A0.6626320.3916920.8766040.090*
H35B0.5341320.3804660.8487290.090*
H35C0.6054000.4363190.8277590.090*
C360.7728 (3)0.37658 (14)0.78161 (16)0.0591 (8)
H36A0.7740190.4181860.7697070.089*
H36B0.8007740.3521260.7494940.089*
H36C0.8225490.3709730.8182890.089*
C370.4609 (2)0.23168 (10)0.91961 (10)0.0309 (5)
C380.40735 (19)0.23783 (10)0.97704 (10)0.0295 (5)
C390.4304 (2)0.19653 (11)1.02244 (11)0.0340 (5)
H390.4830560.1652311.0169640.041*
C400.3760 (2)0.20130 (12)1.07596 (11)0.0373 (6)
H400.3916510.1732561.1070220.045*
C410.2993 (2)0.24693 (12)1.08378 (12)0.0406 (6)
H410.2608170.2495981.1198310.049*
C420.2786 (2)0.28863 (11)1.03920 (12)0.0404 (6)
H420.2273030.3204161.0451540.048*
C430.3320 (2)0.28430 (10)0.98602 (11)0.0339 (5)
H430.3174070.3130530.9555460.041*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0254 (2)0.0215 (2)0.0296 (2)0.00267 (16)0.00727 (16)0.00238 (16)
Ti20.0371 (2)0.0234 (2)0.0287 (2)0.00878 (17)0.00751 (18)0.00126 (16)
N10.0452 (12)0.0255 (10)0.0395 (11)0.0056 (9)0.0114 (10)0.0026 (8)
N20.0449 (13)0.0267 (10)0.0380 (11)0.0080 (9)0.0111 (9)0.0013 (9)
N30.0306 (10)0.0238 (9)0.0343 (11)0.0031 (8)0.0065 (8)0.0029 (8)
N40.0278 (10)0.0234 (9)0.0393 (11)0.0027 (8)0.0086 (8)0.0031 (8)
N50.0279 (10)0.0323 (11)0.0452 (12)0.0003 (8)0.0082 (9)0.0038 (9)
N60.0316 (11)0.0298 (10)0.0317 (10)0.0048 (8)0.0093 (8)0.0001 (8)
N70.0331 (11)0.0247 (10)0.0322 (10)0.0001 (8)0.0064 (8)0.0032 (8)
N80.0283 (10)0.0238 (9)0.0328 (10)0.0033 (8)0.0080 (8)0.0007 (8)
N90.0293 (10)0.0232 (9)0.0334 (10)0.0027 (8)0.0074 (8)0.0005 (8)
N100.0329 (11)0.0216 (9)0.0445 (12)0.0035 (8)0.0087 (9)0.0005 (8)
N110.0298 (10)0.0253 (10)0.0363 (11)0.0003 (8)0.0055 (8)0.0019 (8)
N120.0285 (10)0.0236 (9)0.0294 (10)0.0017 (7)0.0069 (8)0.0003 (7)
N130.0307 (10)0.0269 (9)0.0272 (10)0.0042 (8)0.0099 (8)0.0024 (8)
N140.0382 (12)0.0322 (11)0.0427 (12)0.0024 (9)0.0170 (9)0.0045 (9)
N150.0354 (11)0.0307 (10)0.0377 (11)0.0087 (9)0.0047 (9)0.0048 (9)
N160.0310 (10)0.0254 (10)0.0350 (11)0.0066 (8)0.0011 (8)0.0034 (8)
N170.0414 (12)0.0339 (11)0.0334 (11)0.0128 (9)0.0040 (9)0.0084 (9)
N180.0565 (15)0.0464 (13)0.0396 (12)0.0242 (11)0.0136 (11)0.0179 (10)
N190.0464 (13)0.0329 (11)0.0367 (11)0.0171 (9)0.0132 (10)0.0027 (9)
N200.0616 (15)0.0307 (11)0.0413 (12)0.0049 (10)0.0015 (11)0.0069 (9)
N210.0788 (17)0.0303 (11)0.0289 (11)0.0099 (11)0.0141 (11)0.0006 (9)
N220.100 (2)0.0281 (11)0.0300 (11)0.0193 (12)0.0181 (12)0.0036 (9)
N230.0528 (13)0.0271 (10)0.0290 (10)0.0103 (9)0.0088 (9)0.0022 (8)
N240.0345 (11)0.0274 (10)0.0324 (10)0.0037 (8)0.0073 (8)0.0039 (8)
N250.069 (6)0.028 (3)0.031 (3)0.006 (4)0.015 (4)0.000 (2)
C440.086 (9)0.044 (3)0.076 (5)0.010 (4)0.010 (4)0.009 (3)
C450.090 (7)0.047 (4)0.054 (5)0.006 (4)0.003 (4)0.013 (3)
N25A0.054 (5)0.019 (3)0.034 (3)0.004 (4)0.014 (4)0.003 (2)
C44A0.054 (6)0.037 (3)0.051 (4)0.005 (3)0.007 (3)0.004 (3)
C45A0.064 (7)0.034 (4)0.044 (5)0.001 (5)0.020 (5)0.004 (4)
C10.0231 (11)0.0243 (11)0.0401 (13)0.0002 (9)0.0075 (10)0.0033 (9)
C20.0305 (13)0.0231 (11)0.0504 (15)0.0002 (9)0.0122 (11)0.0038 (10)
C30.0414 (15)0.0259 (12)0.0605 (17)0.0023 (11)0.0235 (13)0.0034 (12)
C40.0455 (16)0.0229 (12)0.073 (2)0.0034 (11)0.0225 (14)0.0068 (12)
C50.0575 (18)0.0273 (13)0.077 (2)0.0080 (12)0.0314 (16)0.0080 (13)
C60.103 (3)0.0346 (15)0.071 (2)0.0136 (17)0.047 (2)0.0046 (15)
C70.083 (2)0.0271 (13)0.0564 (18)0.0120 (14)0.0319 (16)0.0005 (12)
C80.0315 (14)0.0386 (15)0.073 (2)0.0040 (11)0.0162 (13)0.0062 (13)
C90.0368 (15)0.0445 (16)0.0636 (19)0.0095 (12)0.0047 (13)0.0083 (14)
C100.0373 (14)0.0418 (14)0.0310 (13)0.0032 (11)0.0033 (10)0.0040 (11)
C110.0464 (16)0.0431 (14)0.0370 (14)0.0054 (12)0.0122 (12)0.0037 (11)
C120.0296 (12)0.0234 (11)0.0343 (12)0.0011 (9)0.0030 (10)0.0010 (9)
C130.041 (4)0.019 (3)0.026 (3)0.003 (3)0.001 (2)0.003 (2)
C140.049 (4)0.035 (2)0.035 (2)0.001 (2)0.011 (3)0.0024 (18)
C150.063 (5)0.036 (2)0.037 (2)0.010 (2)0.016 (3)0.0005 (18)
C160.078 (5)0.032 (3)0.041 (3)0.005 (3)0.002 (3)0.007 (2)
C170.074 (4)0.025 (3)0.056 (5)0.010 (3)0.012 (4)0.003 (3)
C180.055 (4)0.032 (3)0.039 (3)0.007 (3)0.011 (3)0.001 (2)
C13A0.023 (5)0.033 (5)0.041 (5)0.002 (4)0.011 (4)0.004 (4)
C14A0.057 (7)0.023 (3)0.037 (4)0.006 (3)0.002 (4)0.003 (2)
C15A0.059 (8)0.035 (4)0.038 (4)0.001 (4)0.003 (4)0.004 (3)
C16A0.050 (6)0.018 (3)0.059 (6)0.001 (3)0.002 (4)0.014 (3)
C17A0.063 (6)0.023 (4)0.065 (6)0.001 (4)0.024 (5)0.001 (3)
C18A0.042 (5)0.024 (3)0.044 (5)0.001 (3)0.014 (4)0.002 (3)
C190.0326 (13)0.0268 (12)0.0445 (14)0.0014 (10)0.0122 (11)0.0038 (10)
C200.039 (6)0.037 (6)0.055 (7)0.008 (5)0.009 (5)0.009 (5)
C210.026 (5)0.040 (5)0.069 (7)0.000 (4)0.000 (4)0.008 (5)
C220.034 (5)0.039 (5)0.091 (8)0.006 (4)0.005 (5)0.005 (5)
C230.033 (4)0.050 (5)0.096 (9)0.005 (4)0.010 (5)0.015 (5)
C240.044 (5)0.057 (6)0.116 (9)0.003 (4)0.032 (5)0.010 (5)
C250.045 (5)0.048 (5)0.101 (8)0.008 (4)0.036 (5)0.001 (5)
C20A0.033 (6)0.035 (6)0.046 (7)0.001 (5)0.008 (4)0.014 (4)
C21A0.024 (5)0.033 (5)0.059 (7)0.010 (4)0.001 (4)0.011 (5)
C22A0.027 (5)0.050 (5)0.076 (8)0.008 (4)0.001 (5)0.012 (5)
C23A0.032 (6)0.060 (7)0.092 (8)0.018 (5)0.014 (6)0.018 (5)
C24A0.034 (5)0.074 (8)0.094 (7)0.011 (6)0.021 (5)0.007 (7)
C25A0.040 (6)0.053 (6)0.066 (7)0.006 (5)0.014 (5)0.009 (5)
C20B0.022 (7)0.026 (7)0.068 (9)0.000 (6)0.006 (6)0.011 (6)
C21B0.021 (7)0.037 (8)0.076 (9)0.005 (6)0.007 (7)0.004 (8)
C22B0.030 (8)0.035 (7)0.095 (9)0.008 (6)0.007 (7)0.010 (7)
C23B0.044 (9)0.075 (10)0.104 (11)0.020 (8)0.006 (7)0.012 (9)
C24B0.056 (8)0.093 (10)0.102 (10)0.026 (7)0.027 (8)0.008 (8)
C25B0.045 (8)0.072 (9)0.086 (9)0.018 (7)0.028 (7)0.003 (7)
C260.0448 (15)0.0326 (13)0.0406 (14)0.0104 (11)0.0092 (12)0.0095 (11)
C270.040 (2)0.025 (3)0.039 (3)0.003 (2)0.008 (2)0.008 (2)
C280.040 (3)0.054 (3)0.038 (2)0.005 (2)0.006 (2)0.006 (2)
C290.036 (2)0.072 (3)0.051 (4)0.002 (2)0.005 (2)0.017 (3)
C300.048 (3)0.049 (3)0.048 (3)0.003 (2)0.017 (3)0.005 (2)
C310.055 (3)0.060 (3)0.038 (2)0.002 (3)0.005 (2)0.010 (2)
C320.043 (3)0.046 (4)0.042 (2)0.006 (3)0.006 (2)0.012 (2)
C27A0.032 (6)0.013 (6)0.031 (6)0.004 (5)0.001 (5)0.000 (5)
C28A0.025 (6)0.065 (10)0.049 (7)0.002 (6)0.003 (5)0.005 (8)
C29A0.038 (7)0.059 (9)0.054 (9)0.003 (6)0.012 (6)0.019 (8)
C30A0.041 (7)0.042 (7)0.046 (8)0.006 (6)0.018 (7)0.014 (7)
C31A0.050 (8)0.042 (7)0.034 (6)0.008 (7)0.010 (6)0.005 (5)
C32A0.034 (6)0.024 (6)0.040 (6)0.010 (5)0.005 (5)0.004 (5)
C330.0415 (15)0.0443 (15)0.0508 (16)0.0159 (12)0.0103 (12)0.0038 (12)
C340.0580 (19)0.0404 (15)0.071 (2)0.0264 (14)0.0309 (16)0.0139 (14)
C350.106 (3)0.0385 (16)0.0374 (15)0.0158 (16)0.0174 (16)0.0089 (12)
C360.0516 (19)0.0499 (18)0.074 (2)0.0017 (14)0.0085 (16)0.0216 (16)
C370.0333 (13)0.0282 (12)0.0312 (12)0.0027 (10)0.0019 (10)0.0025 (10)
C380.0266 (12)0.0309 (12)0.0312 (12)0.0049 (9)0.0026 (9)0.0061 (9)
C390.0302 (12)0.0403 (14)0.0316 (12)0.0019 (10)0.0018 (10)0.0020 (10)
C400.0363 (14)0.0461 (15)0.0292 (12)0.0108 (11)0.0004 (10)0.0002 (11)
C410.0358 (14)0.0490 (15)0.0386 (14)0.0154 (12)0.0149 (11)0.0118 (12)
C420.0333 (14)0.0359 (14)0.0536 (16)0.0055 (11)0.0152 (12)0.0069 (12)
C430.0317 (13)0.0306 (12)0.0398 (14)0.0046 (10)0.0057 (10)0.0000 (10)
Geometric parameters (Å, º) top
Ti1—N32.1534 (19)C17—H170.9500
Ti1—N51.892 (2)C17—C181.3900
Ti1—N61.893 (2)C18—H180.9500
Ti1—N82.1967 (18)C13A—C14A1.3900
Ti1—N122.2592 (19)C13A—C18A1.3900
Ti1—N162.294 (2)C14A—H14A0.9500
Ti2—N92.1970 (19)C14A—C15A1.3900
Ti2—N132.2404 (19)C15A—H15A0.9500
Ti2—N172.266 (2)C15A—C16A1.3900
Ti2—N191.901 (2)C16A—H16A0.9500
Ti2—N201.890 (2)C16A—C17A1.3900
Ti2—N232.151 (2)C17A—H17A0.9500
N1—N21.333 (3)C17A—C18A1.3900
N1—C11.350 (3)C18A—H18A0.9500
N2—N31.324 (3)C19—C201.471 (5)
N3—N41.346 (3)C19—C20A1.481 (6)
N4—C11.331 (3)C19—C20B1.477 (7)
N5—C81.449 (3)C20—C211.3900
N5—C91.459 (3)C20—C251.3900
N6—C101.468 (3)C21—H210.9500
N6—C111.460 (3)C21—C221.3900
N7—N81.332 (3)C22—H220.9500
N7—C121.342 (3)C22—C231.3900
N8—N91.333 (2)C23—H230.9500
N9—N101.338 (3)C23—C241.3900
N10—C121.337 (3)C24—H240.9500
N11—N121.329 (3)C24—C251.3900
N11—C191.335 (3)C25—H250.9500
N12—N131.333 (2)C20A—C21A1.3900
N13—N141.333 (3)C20A—C25A1.3900
N14—C191.339 (3)C21A—H21A0.9500
N15—N161.337 (3)C21A—C22A1.3900
N15—C261.336 (3)C22A—H22A0.9500
N16—N171.332 (3)C22A—C23A1.3900
N17—N181.328 (3)C23A—H23A0.9500
N18—C261.337 (3)C23A—C24A1.3900
N19—C331.461 (4)C24A—H24A0.9500
N19—C341.460 (3)C24A—C25A1.3900
N20—C351.464 (3)C25A—H25A0.9500
N20—C361.447 (4)C20B—C21B1.3900
N21—N221.330 (3)C20B—C25B1.3900
N21—C371.345 (3)C21B—H21B0.9500
N22—N231.326 (3)C21B—C22B1.3900
N23—N241.346 (3)C22B—H22B0.9500
N24—C371.336 (3)C22B—C23B1.3900
N25—H25C0.9100C23B—H23B0.9500
N25—H25D0.9100C23B—C24B1.3900
N25—C441.485 (10)C24B—H24B0.9500
N25—C451.472 (10)C24B—C25B1.3900
C44—H44A0.9800C25B—H25B0.9500
C44—H44B0.9800C26—C271.482 (4)
C44—H44C0.9800C26—C27A1.477 (7)
C45—H45A0.9800C27—C281.3900
C45—H45B0.9800C27—C321.3900
C45—H45C0.9800C28—H280.9500
N25A—H25E0.9100C28—C291.3900
N25A—H25F0.9100C29—H290.9500
N25A—C44A1.486 (10)C29—C301.3900
N25A—C45A1.474 (11)C30—H300.9500
C44A—H44D0.9800C30—C311.3900
C44A—H44E0.9800C31—H310.9500
C44A—H44F0.9800C31—C321.3900
C45A—H45D0.9800C32—H320.9500
C45A—H45E0.9800C27A—C28A1.3900
C45A—H45F0.9800C27A—C32A1.3900
C1—C21.470 (3)C28A—H28A0.9500
C2—C31.389 (3)C28A—C29A1.3900
C2—C71.377 (4)C29A—H29A0.9500
C3—H30.9500C29A—C30A1.3900
C3—C41.383 (3)C30A—H30A0.9500
C4—H40.9500C30A—C31A1.3900
C4—C51.372 (4)C31A—H31A0.9500
C5—H50.9500C31A—C32A1.3900
C5—C61.383 (4)C32A—H32A0.9500
C6—H60.9500C33—H33A0.9800
C6—C71.388 (4)C33—H33B0.9800
C7—H70.9500C33—H33C0.9800
C8—H8A0.9800C34—H34A0.9800
C8—H8B0.9800C34—H34B0.9800
C8—H8C0.9800C34—H34C0.9800
C9—H9A0.9800C35—H35A0.9800
C9—H9B0.9800C35—H35B0.9800
C9—H9C0.9800C35—H35C0.9800
C10—H10A0.9800C36—H36A0.9800
C10—H10B0.9800C36—H36B0.9800
C10—H10C0.9800C36—H36C0.9800
C11—H11A0.9800C37—C381.471 (3)
C11—H11B0.9800C38—C391.394 (3)
C11—H11C0.9800C38—C431.393 (3)
C12—C131.492 (3)C39—H390.9500
C12—C13A1.453 (5)C39—C401.395 (3)
C13—C141.3900C40—H400.9500
C13—C181.3900C40—C411.385 (4)
C14—H140.9500C41—H410.9500
C14—C151.3900C41—C421.383 (4)
C15—H150.9500C42—H420.9500
C15—C161.3900C42—C431.382 (3)
C16—H160.9500C43—H430.9500
C16—C171.3900
N3—Ti1—N8164.82 (7)C15—C16—C17120.0
N3—Ti1—N1285.77 (7)C17—C16—H16120.0
N3—Ti1—N1685.01 (7)C16—C17—H17120.0
N5—Ti1—N3101.28 (8)C16—C17—C18120.0
N5—Ti1—N697.98 (9)C18—C17—H17120.0
N5—Ti1—N889.83 (8)C13—C18—H18120.0
N5—Ti1—N12162.38 (8)C17—C18—C13120.0
N5—Ti1—N1685.55 (8)C17—C18—H18120.0
N6—Ti1—N391.25 (8)C14A—C13A—C12116.4 (4)
N6—Ti1—N897.48 (8)C14A—C13A—C18A120.0
N6—Ti1—N1297.99 (8)C18A—C13A—C12123.6 (4)
N6—Ti1—N16175.31 (8)C13A—C14A—H14A120.0
N8—Ti1—N1280.75 (7)C13A—C14A—C15A120.0
N8—Ti1—N1685.58 (7)C15A—C14A—H14A120.0
N12—Ti1—N1678.95 (7)C14A—C15A—H15A120.0
N9—Ti2—N1380.25 (7)C14A—C15A—C16A120.0
N9—Ti2—N1786.32 (7)C16A—C15A—H15A120.0
N13—Ti2—N1777.94 (7)C15A—C16A—H16A120.0
N19—Ti2—N999.42 (8)C17A—C16A—C15A120.0
N19—Ti2—N1396.29 (8)C17A—C16A—H16A120.0
N19—Ti2—N17171.14 (9)C16A—C17A—H17A120.0
N19—Ti2—N2390.31 (8)C16A—C17A—C18A120.0
N20—Ti2—N988.58 (9)C18A—C17A—H17A120.0
N20—Ti2—N13162.12 (9)C13A—C18A—H18A120.0
N20—Ti2—N1787.51 (9)C17A—C18A—C13A120.0
N20—Ti2—N1999.30 (10)C17A—C18A—H18A120.0
N20—Ti2—N2399.98 (9)N11—C19—N14111.9 (2)
N23—Ti2—N9165.88 (7)N11—C19—C20128.2 (6)
N23—Ti2—N1388.58 (7)N11—C19—C20A119.2 (6)
N23—Ti2—N1782.90 (8)N11—C19—C20B128.6 (7)
N2—N1—C1104.42 (19)N14—C19—C20119.9 (6)
N3—N2—N1109.57 (18)N14—C19—C20A128.6 (6)
N2—N3—Ti1124.69 (14)N14—C19—C20B118.6 (7)
N2—N3—N4109.68 (17)C21—C20—C19119.2 (9)
N4—N3—Ti1125.62 (14)C21—C20—C25120.0
C1—N4—N3104.27 (18)C25—C20—C19120.8 (9)
C8—N5—Ti1120.62 (17)C20—C21—H21120.0
C8—N5—C9111.0 (2)C22—C21—C20120.0
C9—N5—Ti1128.03 (17)C22—C21—H21120.0
C10—N6—Ti1126.00 (15)C21—C22—H22120.0
C11—N6—Ti1124.70 (17)C23—C22—C21120.0
C11—N6—C10109.2 (2)C23—C22—H22120.0
N8—N7—C12104.28 (17)C22—C23—H23120.0
N7—N8—Ti1119.02 (13)C22—C23—C24120.0
N7—N8—N9109.76 (17)C24—C23—H23120.0
N9—N8—Ti1131.21 (14)C23—C24—H24120.0
N8—N9—Ti2132.47 (14)C25—C24—C23120.0
N8—N9—N10109.22 (17)C25—C24—H24120.0
N10—N9—Ti2118.22 (14)C20—C25—H25120.0
C12—N10—N9104.46 (17)C24—C25—C20120.0
N12—N11—C19104.57 (18)C24—C25—H25120.0
N11—N12—Ti1120.87 (13)C21A—C20A—C19120.8 (9)
N11—N12—N13109.87 (17)C21A—C20A—C25A120.0
N13—N12—Ti1129.04 (14)C25A—C20A—C19118.9 (9)
N12—N13—Ti2132.19 (14)C20A—C21A—H21A120.0
N14—N13—Ti2118.97 (14)C22A—C21A—C20A120.0
N14—N13—N12108.83 (18)C22A—C21A—H21A120.0
N13—N14—C19104.86 (18)C21A—C22A—H22A120.0
C26—N15—N16104.17 (19)C23A—C22A—C21A120.0
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N17—N16—Ti1130.05 (15)C22A—C23A—H23A120.0
N17—N16—N15109.33 (18)C22A—C23A—C24A120.0
N16—N17—Ti2130.06 (15)C24A—C23A—H23A120.0
N18—N17—Ti2119.97 (15)C23A—C24A—H24A120.0
N18—N17—N16109.65 (19)C25A—C24A—C23A120.0
N17—N18—C26104.4 (2)C25A—C24A—H24A120.0
C33—N19—Ti2127.09 (16)C20A—C25A—H25A120.0
C34—N19—Ti2123.05 (19)C24A—C25A—C20A120.0
C34—N19—C33109.8 (2)C24A—C25A—H25A120.0
C35—N20—Ti2120.7 (2)C21B—C20B—C19119.6 (10)
C36—N20—Ti2127.85 (18)C21B—C20B—C25B120.0
C36—N20—C35111.3 (2)C25B—C20B—C19120.0 (10)
N22—N21—C37105.0 (2)C20B—C21B—H21B120.0
N23—N22—N21109.12 (19)C20B—C21B—C22B120.0
N22—N23—Ti2125.74 (15)C22B—C21B—H21B120.0
N22—N23—N24110.03 (19)C21B—C22B—H22B120.0
N24—N23—Ti2124.21 (14)C23B—C22B—C21B120.0
C37—N24—N23103.93 (18)C23B—C22B—H22B120.0
H25C—N25—H25D107.8C22B—C23B—H23B120.0
C44—N25—H25C109.0C22B—C23B—C24B120.0
C44—N25—H25D109.0C24B—C23B—H23B120.0
C45—N25—H25C109.0C23B—C24B—H24B120.0
C45—N25—H25D109.0C25B—C24B—C23B120.0
C45—N25—C44113.0 (6)C25B—C24B—H24B120.0
N25—C44—H44A109.5C20B—C25B—H25B120.0
N25—C44—H44B109.5C24B—C25B—C20B120.0
N25—C44—H44C109.5C24B—C25B—H25B120.0
H44A—C44—H44B109.5N15—C26—N18112.4 (2)
H44A—C44—H44C109.5N15—C26—C27125.8 (3)
H44B—C44—H44C109.5N15—C26—C27A118.2 (8)
N25—C45—H45A109.5N18—C26—C27121.6 (3)
N25—C45—H45B109.5N18—C26—C27A128.3 (8)
N25—C45—H45C109.5C28—C27—C26118.0 (4)
H45A—C45—H45B109.5C28—C27—C32120.0
H45A—C45—H45C109.5C32—C27—C26121.8 (4)
H45B—C45—H45C109.5C27—C28—H28120.0
H25E—N25A—H25F107.5C27—C28—C29120.0
C44A—N25A—H25E108.5C29—C28—H28120.0
C44A—N25A—H25F108.5C28—C29—H29120.0
C45A—N25A—H25E108.5C28—C29—C30120.0
C45A—N25A—H25F108.5C30—C29—H29120.0
C45A—N25A—C44A115.1 (7)C29—C30—H30120.0
N25A—C44A—H44D109.5C31—C30—C29120.0
N25A—C44A—H44E109.5C31—C30—H30120.0
N25A—C44A—H44F109.5C30—C31—H31120.0
H44D—C44A—H44E109.5C30—C31—C32120.0
H44D—C44A—H44F109.5C32—C31—H31120.0
H44E—C44A—H44F109.5C27—C32—H32120.0
N25A—C45A—H45D109.5C31—C32—C27120.0
N25A—C45A—H45E109.5C31—C32—H32120.0
N25A—C45A—H45F109.5C28A—C27A—C26125.5 (10)
H45D—C45A—H45E109.5C28A—C27A—C32A120.0
H45D—C45A—H45F109.5C32A—C27A—C26113.5 (9)
H45E—C45A—H45F109.5C27A—C28A—H28A120.0
N1—C1—C2123.5 (2)C29A—C28A—C27A120.0
N4—C1—N1112.07 (19)C29A—C28A—H28A120.0
N4—C1—C2124.4 (2)C28A—C29A—H29A120.0
C3—C2—C1120.4 (2)C30A—C29A—C28A120.0
C7—C2—C1120.6 (2)C30A—C29A—H29A120.0
C7—C2—C3119.0 (2)C29A—C30A—H30A120.0
C2—C3—H3119.5C29A—C30A—C31A120.0
C4—C3—C2121.0 (2)C31A—C30A—H30A120.0
C4—C3—H3119.5C30A—C31A—H31A120.0
C3—C4—H4120.1C32A—C31A—C30A120.0
C5—C4—C3119.8 (2)C32A—C31A—H31A120.0
C5—C4—H4120.1C27A—C32A—H32A120.0
C4—C5—H5120.1C31A—C32A—C27A120.0
C4—C5—C6119.7 (2)C31A—C32A—H32A120.0
C6—C5—H5120.1N19—C33—H33A109.5
C5—C6—H6119.7N19—C33—H33B109.5
C5—C6—C7120.5 (3)N19—C33—H33C109.5
C7—C6—H6119.7H33A—C33—H33B109.5
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C2—C7—H7120.0H33B—C33—H33C109.5
C6—C7—H7120.0N19—C34—H34A109.5
N5—C8—H8A109.5N19—C34—H34B109.5
N5—C8—H8B109.5N19—C34—H34C109.5
N5—C8—H8C109.5H34A—C34—H34B109.5
H8A—C8—H8B109.5H34A—C34—H34C109.5
H8A—C8—H8C109.5H34B—C34—H34C109.5
H8B—C8—H8C109.5N20—C35—H35A109.5
N5—C9—H9A109.5N20—C35—H35B109.5
N5—C9—H9B109.5N20—C35—H35C109.5
N5—C9—H9C109.5H35A—C35—H35B109.5
H9A—C9—H9B109.5H35A—C35—H35C109.5
H9A—C9—H9C109.5H35B—C35—H35C109.5
H9B—C9—H9C109.5N20—C36—H36A109.5
N6—C10—H10A109.5N20—C36—H36B109.5
N6—C10—H10B109.5N20—C36—H36C109.5
N6—C10—H10C109.5H36A—C36—H36B109.5
H10A—C10—H10B109.5H36A—C36—H36C109.5
H10A—C10—H10C109.5H36B—C36—H36C109.5
H10B—C10—H10C109.5N21—C37—C38124.2 (2)
N6—C11—H11A109.5N24—C37—N21112.0 (2)
N6—C11—H11B109.5N24—C37—C38123.9 (2)
N6—C11—H11C109.5C39—C38—C37120.0 (2)
H11A—C11—H11B109.5C43—C38—C37120.3 (2)
H11A—C11—H11C109.5C43—C38—C39119.7 (2)
H11B—C11—H11C109.5C38—C39—H39120.1
N7—C12—C13120.6 (3)C38—C39—C40119.8 (2)
N7—C12—C13A130.3 (3)C40—C39—H39120.1
N10—C12—N7112.27 (19)C39—C40—H40120.0
N10—C12—C13127.1 (3)C41—C40—C39120.0 (2)
N10—C12—C13A117.4 (3)C41—C40—H40120.0
C14—C13—C12122.6 (3)C40—C41—H41119.9
C14—C13—C18120.0C42—C41—C40120.1 (2)
C18—C13—C12117.3 (3)C42—C41—H41119.9
C13—C14—H14120.0C41—C42—H42119.8
C13—C14—C15120.0C43—C42—C41120.3 (2)
C15—C14—H14120.0C43—C42—H42119.8
C14—C15—H15120.0C38—C43—H43119.9
C16—C15—C14120.0C42—C43—C38120.1 (2)
C16—C15—H15120.0C42—C43—H43119.9
C15—C16—H16120.0
Ti1—N3—N4—C1178.70 (15)N18—C26—C27—C28148.5 (4)
Ti1—N8—N9—Ti25.1 (3)N18—C26—C27—C3227.4 (5)
Ti1—N8—N9—N10178.59 (15)N18—C26—C27A—C28A159.1 (8)
Ti1—N12—N13—Ti26.7 (3)N18—C26—C27A—C32A32.0 (15)
Ti1—N12—N13—N14174.66 (15)N19—Ti2—N20—C3541.5 (2)
Ti1—N16—N17—Ti20.9 (3)N19—Ti2—N20—C36142.7 (2)
Ti1—N16—N17—N18172.50 (17)N21—N22—N23—Ti2178.79 (18)
Ti2—N9—N10—C12176.63 (15)N21—N22—N23—N240.5 (3)
Ti2—N13—N14—C19178.54 (15)N21—C37—C38—C3920.1 (4)
Ti2—N17—N18—C26174.34 (18)N21—C37—C38—C43158.9 (2)
Ti2—N23—N24—C37178.31 (17)N22—N21—C37—N240.8 (3)
N1—N2—N3—Ti1178.75 (15)N22—N21—C37—C38179.6 (2)
N1—N2—N3—N40.1 (3)N22—N23—N24—C370.0 (3)
N1—C1—C2—C310.2 (4)N23—Ti2—N20—C3550.4 (2)
N1—C1—C2—C7172.1 (3)N23—Ti2—N20—C36125.3 (2)
N2—N1—C1—N40.0 (3)N23—N24—C37—N210.5 (3)
N2—N1—C1—C2179.0 (2)N23—N24—C37—C38179.3 (2)
N2—N3—N4—C10.0 (2)N24—C37—C38—C39161.3 (2)
N3—Ti1—N5—C846.1 (2)N24—C37—C38—C4319.7 (4)
N3—Ti1—N5—C9126.9 (2)C1—N1—N2—N30.1 (3)
N3—Ti1—N6—C1044.08 (19)C1—C2—C3—C4177.5 (2)
N3—Ti1—N6—C11132.57 (19)C1—C2—C7—C6176.7 (3)
N3—N4—C1—N10.0 (3)C2—C3—C4—C50.2 (4)
N3—N4—C1—C2178.9 (2)C3—C2—C7—C61.0 (5)
N4—C1—C2—C3168.5 (2)C3—C4—C5—C60.2 (5)
N4—C1—C2—C79.1 (4)C4—C5—C6—C71.0 (6)
N5—Ti1—N6—C10145.65 (19)C5—C6—C7—C21.4 (6)
N5—Ti1—N6—C1131.0 (2)C7—C2—C3—C40.2 (4)
N6—Ti1—N5—C846.8 (2)C12—N7—N8—Ti1178.60 (14)
N6—Ti1—N5—C9140.2 (2)C12—N7—N8—N90.8 (2)
N7—N8—N9—Ti2175.61 (15)C12—C13—C14—C15177.9 (4)
N7—N8—N9—N100.7 (2)C12—C13—C18—C17178.0 (4)
N7—C12—C13—C149.2 (5)C12—C13A—C14A—C15A178.4 (6)
N7—C12—C13—C18172.9 (3)C12—C13A—C18A—C17A178.2 (6)
N7—C12—C13A—C14A20.4 (7)C13—C14—C15—C160.0
N7—C12—C13A—C18A161.3 (5)C14—C13—C18—C170.0
N8—Ti1—N5—C8144.4 (2)C14—C15—C16—C170.0
N8—Ti1—N5—C942.7 (2)C15—C16—C17—C180.0
N8—Ti1—N6—C10123.46 (18)C16—C17—C18—C130.0
N8—Ti1—N6—C1159.88 (19)C18—C13—C14—C150.0
N8—N7—C12—N100.6 (3)C13A—C14A—C15A—C16A0.0
N8—N7—C12—C13179.2 (3)C14A—C13A—C18A—C17A0.0
N8—N7—C12—C13A178.7 (4)C14A—C15A—C16A—C17A0.0
N8—N9—N10—C120.3 (2)C15A—C16A—C17A—C18A0.0
N9—Ti2—N20—C35140.9 (2)C16A—C17A—C18A—C13A0.0
N9—Ti2—N20—C3643.4 (2)C18A—C13A—C14A—C15A0.0
N9—N10—C12—N70.2 (3)C19—N11—N12—Ti1175.55 (15)
N9—N10—C12—C13179.6 (3)C19—N11—N12—N130.5 (2)
N9—N10—C12—C13A179.2 (3)C19—C20—C21—C22179.1 (13)
N10—C12—C13—C14170.9 (4)C19—C20—C25—C24179.1 (13)
N10—C12—C13—C187.0 (5)C19—C20A—C21A—C22A173.9 (15)
N10—C12—C13A—C14A158.9 (5)C19—C20A—C25A—C24A174.0 (15)
N10—C12—C13A—C18A19.4 (7)C19—C20B—C21B—C22B173.1 (15)
N11—N12—N13—Ti2178.75 (15)C19—C20B—C25B—C24B173.1 (15)
N11—N12—N13—N140.1 (2)C20—C21—C22—C230.0
N11—C19—C20—C219.3 (15)C21—C20—C25—C240.0
N11—C19—C20—C25169.8 (6)C21—C22—C23—C240.0
N11—C19—C20A—C21A6.6 (13)C22—C23—C24—C250.0
N11—C19—C20A—C25A179.4 (6)C23—C24—C25—C200.0
N11—C19—C20B—C21B30.6 (13)C25—C20—C21—C220.0
N11—C19—C20B—C25B156.3 (8)C20A—C21A—C22A—C23A0.0
N12—Ti1—N5—C8158.3 (2)C21A—C20A—C25A—C24A0.0
N12—Ti1—N5—C914.6 (4)C21A—C22A—C23A—C24A0.0
N12—Ti1—N6—C1041.82 (19)C22A—C23A—C24A—C25A0.0
N12—Ti1—N6—C11141.53 (18)C23A—C24A—C25A—C20A0.0
N12—N11—C19—N140.7 (3)C25A—C20A—C21A—C22A0.0
N12—N11—C19—C20178.4 (9)C20B—C21B—C22B—C23B0.0
N12—N11—C19—C20A172.9 (9)C21B—C20B—C25B—C24B0.0
N12—N11—C19—C20B169.3 (10)C21B—C22B—C23B—C24B0.0
N12—N13—N14—C190.3 (2)C22B—C23B—C24B—C25B0.0
N13—Ti2—N20—C35168.1 (2)C23B—C24B—C25B—C20B0.0
N13—Ti2—N20—C367.7 (4)C25B—C20B—C21B—C22B0.0
N13—N14—C19—N110.6 (3)C26—N15—N16—Ti1173.39 (16)
N13—N14—C19—C20178.5 (8)C26—N15—N16—N170.2 (3)
N13—N14—C19—C20A172.2 (10)C26—C27—C28—C29176.0 (6)
N13—N14—C19—C20B170.5 (9)C26—C27—C32—C31175.8 (6)
N14—C19—C20—C21171.7 (6)C26—C27A—C28A—C29A168.2 (15)
N14—C19—C20—C259.2 (11)C26—C27A—C32A—C31A169.5 (14)
N14—C19—C20A—C21A179.0 (6)C27—C28—C29—C300.0
N14—C19—C20A—C25A7.0 (13)C28—C27—C32—C310.0
N14—C19—C20B—C21B161.4 (8)C28—C29—C30—C310.0
N14—C19—C20B—C25B11.7 (15)C29—C30—C31—C320.0
N15—N16—N17—Ti2173.61 (16)C30—C31—C32—C270.0
N15—N16—N17—N180.2 (3)C32—C27—C28—C290.0
N15—C26—C27—C2837.5 (8)C27A—C28A—C29A—C30A0.0
N15—C26—C27—C32146.6 (5)C28A—C27A—C32A—C31A0.0
N15—C26—C27A—C28A8.6 (14)C28A—C29A—C30A—C31A0.0
N15—C26—C27A—C32A160.2 (9)C29A—C30A—C31A—C32A0.0
N16—Ti1—N5—C8130.1 (2)C30A—C31A—C32A—C27A0.0
N16—Ti1—N5—C942.9 (2)C32A—C27A—C28A—C29A0.0
N16—N15—C26—N180.1 (3)C37—N21—N22—N230.8 (3)
N16—N15—C26—C27174.6 (5)C37—C38—C39—C40177.6 (2)
N16—N15—C26—C27A169.5 (9)C37—C38—C43—C42177.6 (2)
N16—N17—N18—C260.2 (3)C38—C39—C40—C410.1 (4)
N17—Ti2—N20—C35132.8 (2)C39—C38—C43—C421.4 (4)
N17—Ti2—N20—C3642.9 (2)C39—C40—C41—C421.6 (4)
N17—N18—C26—N150.1 (3)C40—C41—C42—C431.6 (4)
N17—N18—C26—C27174.7 (5)C41—C42—C43—C380.1 (4)
N17—N18—C26—C27A168.4 (10)C43—C38—C39—C401.4 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N25—H25C···N220.911.892.742 (7)156
N25—H25D···N20.911.972.864 (8)169
N25A—H25E···N220.912.002.847 (8)154
N25A—H25F···N20.911.822.690 (8)160
Bis(dimethylamido)-1κN,2κN-bis(dimethylamine)-1κN,2κN-tris(µ-5-phenyltetrazolato-1:2κ2N2:N3)tris(5-phenyltetrazolato)-1κ2N2;2κ2N2,N3- dizirconium(III)]–benzene–dichloromethane (1/1.12/0.38) (2) top
Crystal data top
[Zr2(C7H5N4)6(C2H6N)2(C2H7N)2]·1.118C6H6·0.382CH2Cl2Z = 4
Mr = 1351.41F(000) = 2780
Triclinic, P1Dx = 1.424 Mg m3
a = 13.9631 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 16.7619 (6) ÅCell parameters from 7364 reflections
c = 27.3054 (9) Åθ = 2.3–26.4°
α = 86.902 (1)°µ = 0.43 mm1
β = 81.154 (1)°T = 100 K
γ = 89.969 (1)°Block, black
V = 6305.3 (4) Å30.4 × 0.3 × 0.2 mm
Data collection top
Bruker SMART APEX CCD area detector
diffractometer
20488 reflections with I > 2σ(I)
φ and ω scansRint = 0.040
Absorption correction: multi-scan
(SADABS; Bruker, 2018)
θmax = 26.4°, θmin = 1.6°
Tmin = 0.578, Tmax = 0.745h = 1717
70012 measured reflectionsk = 2020
25682 independent reflectionsl = 3434
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.039H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.103 w = 1/[σ2(Fo2) + (0.0515P)2 + 3.6611P]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.002
25682 reflectionsΔρmax = 0.78 e Å3
1671 parametersΔρmin = 0.98 e Å3
67 restraints
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr10.61268 (2)0.30119 (2)0.47371 (2)0.01542 (6)
Zr20.34460 (2)0.20179 (2)0.42388 (2)0.01759 (6)
N10.62854 (13)0.22073 (11)0.58320 (7)0.0208 (4)
N20.60391 (13)0.20746 (11)0.53866 (7)0.0192 (4)
N30.58410 (14)0.13076 (11)0.53494 (7)0.0234 (4)
N40.59644 (14)0.09241 (11)0.57734 (7)0.0247 (4)
N50.80075 (14)0.31034 (12)0.38630 (7)0.0229 (4)
N60.70385 (13)0.31597 (11)0.39458 (7)0.0199 (4)
N70.66779 (14)0.30315 (12)0.35321 (7)0.0241 (4)
N80.74034 (14)0.28880 (13)0.31795 (7)0.0280 (5)
N90.63792 (14)0.41426 (11)0.48542 (7)0.0210 (4)
N100.77681 (14)0.27429 (11)0.48624 (7)0.0201 (4)
H100.8031 (17)0.2918 (15)0.4576 (7)0.024*
N110.41333 (13)0.31161 (11)0.55967 (7)0.0217 (4)
N120.44930 (13)0.28982 (11)0.51454 (7)0.0194 (4)
N130.38227 (14)0.25117 (11)0.49607 (7)0.0216 (4)
N140.30044 (14)0.24728 (11)0.52818 (7)0.0230 (4)
N150.52088 (13)0.42456 (11)0.39744 (7)0.0184 (4)
N160.50747 (13)0.35138 (10)0.41900 (7)0.0174 (4)
N170.43992 (13)0.31375 (11)0.39964 (7)0.0179 (4)
N180.40824 (13)0.36086 (11)0.36503 (7)0.0191 (4)
N190.65646 (13)0.14180 (11)0.41511 (7)0.0206 (4)
N200.58099 (13)0.18582 (11)0.43214 (7)0.0192 (4)
N210.50045 (13)0.15249 (11)0.42243 (7)0.0187 (4)
N220.52220 (13)0.08542 (11)0.39893 (7)0.0202 (4)
N230.21105 (13)0.28332 (11)0.42890 (7)0.0211 (4)
N240.18528 (14)0.20888 (11)0.44746 (7)0.0232 (4)
N250.09398 (14)0.20583 (12)0.46739 (8)0.0286 (5)
N260.05718 (14)0.27850 (13)0.46227 (8)0.0300 (5)
N270.32391 (14)0.07081 (11)0.45608 (7)0.0210 (4)
H270.3670 (16)0.0447 (14)0.4388 (9)0.025*
N280.36740 (14)0.18038 (11)0.35261 (7)0.0226 (4)
C10.62307 (16)0.14830 (13)0.60612 (8)0.0205 (5)
C20.64476 (17)0.13144 (14)0.65660 (9)0.0245 (5)
C30.68779 (19)0.18972 (15)0.68025 (9)0.0294 (6)
H30.7033950.2404130.6636750.035*
C40.7082 (2)0.17444 (17)0.72797 (10)0.0363 (6)
H40.7373490.2146070.7441620.044*
C50.6858 (2)0.10033 (18)0.75192 (10)0.0396 (7)
H50.6999610.0896550.7845650.048*
C60.6433 (2)0.04215 (17)0.72872 (10)0.0386 (7)
H60.6281190.0085280.7454010.046*
C70.62236 (18)0.05710 (15)0.68105 (9)0.0298 (6)
H70.5928660.0167920.6651150.036*
C80.82114 (17)0.29256 (14)0.33908 (8)0.0236 (5)
C90.91872 (18)0.27617 (15)0.31423 (9)0.0266 (5)
C100.9320 (2)0.22943 (19)0.27315 (10)0.0391 (7)
H10A0.8773080.2097490.2606020.047*
C111.0243 (2)0.2115 (2)0.25055 (11)0.0468 (8)
H111.0328760.1790910.2227610.056*
C121.1038 (2)0.24065 (19)0.26823 (10)0.0414 (7)
H121.1672780.2286650.2524580.050*
C131.09133 (19)0.28737 (18)0.30897 (10)0.0368 (6)
H131.1462950.3076830.3209910.044*
C140.99937 (18)0.30453 (15)0.33219 (10)0.0302 (6)
H140.9911630.3358000.3605150.036*
C150.61138 (17)0.42062 (14)0.53901 (9)0.0253 (5)
H15A0.5568370.4573400.5455660.038*
H15B0.6669140.4409870.5526880.038*
H15C0.5926140.3677990.5546750.038*
C160.6714 (2)0.48938 (15)0.45970 (10)0.0322 (6)
H16A0.6885320.4816040.4241220.048*
H16B0.7284140.5082700.4727020.048*
H16C0.6197240.5290580.4648930.048*
C170.81005 (17)0.19055 (14)0.49107 (9)0.0240 (5)
H17A0.7840730.1672610.5241320.036*
H17B0.8810370.1896480.4864940.036*
H17C0.7870000.1594300.4657700.036*
C180.81420 (16)0.32087 (14)0.52359 (9)0.0230 (5)
H18A0.8076650.3780370.5153200.034*
H18B0.8826840.3083210.5238330.034*
H18C0.7771000.3072160.5564390.034*
C190.32131 (16)0.28518 (13)0.56707 (9)0.0222 (5)
C200.24926 (17)0.29685 (15)0.61158 (9)0.0273 (5)
C210.2758 (2)0.33139 (18)0.65243 (11)0.0449 (8)
H210.3408650.3486420.6517360.054*
C220.2078 (3)0.3409 (2)0.69446 (13)0.0580 (10)
H220.2265000.3644960.7224450.070*
C230.1142 (2)0.31654 (19)0.69568 (13)0.0534 (9)
H230.0676240.3233990.7243760.064*
C240.0873 (2)0.28183 (19)0.65500 (12)0.0465 (8)
H240.0221100.2649040.6559450.056*
C250.15409 (19)0.27145 (17)0.61302 (11)0.0376 (6)
H250.1351240.2471380.5853400.045*
C260.45857 (16)0.42866 (13)0.36455 (8)0.0184 (4)
C270.44358 (15)0.49932 (13)0.33280 (8)0.0193 (5)
C280.39002 (16)0.49213 (14)0.29410 (8)0.0222 (5)
H280.3644710.4415740.2883190.027*
C290.37408 (17)0.55839 (14)0.26418 (9)0.0258 (5)
H290.3375340.5532960.2378880.031*
C300.41116 (18)0.63209 (15)0.27240 (9)0.0273 (5)
H300.4005300.6774720.2515980.033*
C310.46386 (18)0.63978 (14)0.31100 (9)0.0261 (5)
H310.4885490.6905930.3169020.031*
C320.48054 (16)0.57368 (13)0.34089 (9)0.0218 (5)
H320.5173700.5790340.3670400.026*
C330.61834 (16)0.08062 (13)0.39496 (8)0.0184 (4)
C340.67460 (17)0.01661 (14)0.36960 (8)0.0225 (5)
C350.77428 (19)0.02168 (17)0.35880 (11)0.0397 (7)
H350.8076640.0663660.3682200.048*
C360.8254 (2)0.0390 (2)0.33407 (14)0.0563 (10)
H360.8941430.0360730.3270020.068*
C370.7778 (2)0.10332 (19)0.31972 (13)0.0502 (8)
H370.8133400.1441040.3022990.060*
C380.6789 (2)0.10855 (16)0.33056 (11)0.0379 (7)
H380.6459190.1532210.3208520.046*
C390.62687 (19)0.04890 (15)0.35562 (10)0.0293 (5)
H390.5582790.0528950.3632640.035*
C400.12978 (16)0.32573 (14)0.43856 (9)0.0225 (5)
C410.11764 (17)0.41034 (14)0.42446 (9)0.0234 (5)
C420.03013 (19)0.44829 (16)0.43942 (10)0.0342 (6)
H420.0212700.4195450.4596620.041*
C430.0174 (2)0.52724 (17)0.42509 (11)0.0384 (7)
H430.0428290.5524100.4351790.046*
C440.09181 (19)0.56970 (15)0.39622 (10)0.0313 (6)
H440.0830710.6242060.3865930.038*
C450.17932 (18)0.53285 (15)0.38124 (9)0.0285 (5)
H450.2307310.5622350.3614400.034*
C460.19222 (17)0.45358 (14)0.39496 (9)0.0253 (5)
H460.2521950.4284240.3842220.030*
C470.22943 (18)0.03270 (15)0.45250 (11)0.0339 (6)
H47A0.1774290.0597080.4734960.051*
H47B0.2306620.0237850.4636840.051*
H47C0.2178380.0370370.4179620.051*
C480.3456 (2)0.05685 (15)0.50735 (9)0.0310 (6)
H48A0.4102000.0782380.5092430.047*
H48B0.3439220.0006470.5161610.047*
H48C0.2971580.0837400.5305210.047*
C490.2814 (2)0.15562 (18)0.33299 (11)0.0402 (7)
H49A0.2916530.1023470.3200830.060*
H49B0.2693830.1937450.3061650.060*
H49C0.2254630.1541190.3595240.060*
C500.45123 (19)0.18986 (16)0.31334 (9)0.0310 (6)
H50A0.4364900.2291910.2877230.047*
H50B0.4661210.1384400.2985650.047*
H50C0.5072290.2083000.3274200.047*
Zr1A0.37957 (2)0.70314 (2)0.04253 (2)0.01696 (6)
Zr2A0.64966 (2)0.80361 (2)0.09192 (2)0.01925 (6)
N1A0.36150 (14)0.77776 (11)0.06673 (7)0.0221 (4)
N2A0.38650 (13)0.79473 (11)0.02306 (7)0.0217 (4)
N3A0.41342 (14)0.87049 (11)0.02291 (7)0.0238 (4)
N4A0.40542 (15)0.90441 (12)0.06726 (7)0.0253 (4)
N5A0.20531 (14)0.64040 (12)0.12747 (7)0.0235 (4)
N6A0.28677 (14)0.68526 (11)0.11991 (7)0.0215 (4)
N7A0.31114 (14)0.70497 (12)0.16280 (7)0.0251 (4)
N8A0.24647 (14)0.67307 (12)0.19905 (7)0.0252 (4)
N9A0.36279 (14)0.59105 (12)0.02498 (8)0.0271 (5)
N10A0.21364 (14)0.72782 (12)0.03220 (7)0.0230 (4)
H10B0.1874 (17)0.7119 (15)0.0611 (7)0.028*
N11A0.47335 (14)0.58276 (11)0.12085 (7)0.0230 (4)
N12A0.48419 (13)0.65560 (11)0.09910 (7)0.0207 (4)
N13A0.55103 (13)0.69500 (11)0.11788 (7)0.0204 (4)
N14A0.58527 (13)0.64884 (11)0.15251 (7)0.0218 (4)
N15A0.57138 (14)0.68622 (11)0.04041 (7)0.0231 (4)
N16A0.54249 (13)0.71614 (11)0.00336 (7)0.0207 (4)
N17A0.61683 (14)0.74946 (11)0.01917 (7)0.0225 (4)
N18A0.69654 (14)0.74154 (12)0.01383 (7)0.0238 (4)
N19A0.34077 (14)0.86992 (11)0.09398 (7)0.0216 (4)
N20A0.41367 (13)0.82036 (11)0.08255 (7)0.0198 (4)
N21A0.49519 (13)0.85353 (11)0.09094 (7)0.0196 (4)
N22A0.47646 (14)0.92570 (11)0.10816 (7)0.0213 (4)
N23A0.77778 (14)0.71751 (12)0.08384 (7)0.0234 (4)
N24A0.80739 (14)0.79207 (12)0.06710 (7)0.0253 (4)
N25A0.89672 (15)0.79183 (14)0.04436 (8)0.0334 (5)
N26A0.92812 (15)0.71682 (14)0.04562 (9)0.0354 (5)
N27A0.67541 (15)0.93016 (12)0.05386 (8)0.0244 (4)
H27A0.6310 (16)0.9604 (14)0.0670 (10)0.029*
N28A0.63770 (15)0.82844 (12)0.16301 (8)0.0281 (5)
C1A0.37409 (16)0.84700 (13)0.09319 (8)0.0202 (5)
C21A0.51900 (18)0.43569 (15)0.17568 (10)0.0299 (6)
H21A0.4821130.4308540.1494990.036*
C2A0.35484 (17)0.85862 (15)0.14460 (9)0.0243 (5)
C3A0.31896 (18)0.79562 (16)0.16750 (10)0.0302 (6)
H3A0.3066800.7453320.1498690.036*
C4A0.3010 (2)0.80564 (18)0.21580 (10)0.0368 (6)
H4A0.2757700.7624080.2311240.044*
C5A0.3195 (2)0.87799 (19)0.24179 (10)0.0418 (7)
H5A0.3078110.8843800.2751380.050*
C6A0.3550 (2)0.94122 (18)0.21960 (10)0.0406 (7)
H6A0.3671360.9912020.2376020.049*
C7A0.37299 (19)0.93208 (16)0.17083 (9)0.0312 (6)
H7A0.3975090.9756750.1555440.037*
C8A0.18268 (16)0.63352 (13)0.17671 (8)0.0216 (5)
C9A0.10072 (17)0.58678 (14)0.20418 (9)0.0232 (5)
C10A0.10237 (18)0.55922 (15)0.25292 (9)0.0271 (5)
H10C0.1552840.5729520.2689980.033*
C11A0.02767 (19)0.51193 (15)0.27831 (9)0.0306 (6)
H11A0.0298390.4929100.3115350.037*
C12A0.0499 (2)0.49240 (16)0.25541 (10)0.0341 (6)
H12A0.1006730.4592580.2726460.041*
C13A0.0536 (2)0.52101 (17)0.20758 (10)0.0362 (6)
H13A0.1079570.5087790.1922130.043*
C14A0.02166 (19)0.56767 (16)0.18156 (10)0.0311 (6)
H14A0.0190860.5864880.1483400.037*
C15A0.33493 (19)0.51583 (14)0.05217 (10)0.0309 (6)
H15D0.3879140.4775650.0458790.046*
H15E0.2768070.4946390.0412290.046*
H15F0.3212480.5244360.0877710.046*
C16A0.38255 (19)0.58051 (16)0.02858 (10)0.0328 (6)
H16D0.3979730.6324510.0462680.049*
H16E0.3252640.5575110.0393710.049*
H16F0.4376270.5445260.0358990.049*
C17A0.17900 (18)0.81114 (15)0.02603 (10)0.0293 (6)
H17D0.2034330.8442120.0500090.044*
H17E0.1079750.8114610.0317560.044*
H17F0.2027690.8326610.0077340.044*
C18A0.17712 (17)0.67913 (14)0.00470 (9)0.0270 (5)
H18D0.2136470.6925730.0377140.041*
H18E0.1082600.6902480.0048850.041*
H18F0.1852540.6223250.0040620.041*
C19A0.53665 (16)0.58033 (14)0.15330 (8)0.0217 (5)
C20A0.55593 (17)0.50953 (14)0.18418 (9)0.0240 (5)
C22A0.5357 (2)0.36906 (16)0.20516 (11)0.0360 (6)
H22A0.5095890.3186530.1994860.043*
C23A0.59041 (19)0.37576 (16)0.24297 (10)0.0335 (6)
H23A0.6009260.3301000.2635720.040*
C24A0.62965 (18)0.44862 (15)0.25077 (9)0.0301 (6)
H24A0.6684680.4528300.2762090.036*
C25A0.61248 (17)0.51586 (15)0.22145 (9)0.0254 (5)
H25A0.6393700.5660760.2268820.030*
C26A0.66635 (17)0.70236 (13)0.05005 (8)0.0216 (5)
C27A0.73017 (18)0.67617 (14)0.09393 (9)0.0262 (5)
C28A0.8295 (2)0.67398 (18)0.09588 (10)0.0390 (7)
H28A0.8582200.6911420.0688440.047*
C29A0.8871 (2)0.6467 (2)0.13739 (11)0.0497 (8)
H29A0.9555720.6458900.1389820.060*
C30A0.8459 (2)0.62070 (18)0.17630 (11)0.0485 (8)
H30A0.8859060.6008770.2042870.058*
C31A0.7469 (2)0.62320 (18)0.17502 (11)0.0444 (7)
H31A0.7185260.6059260.2021270.053*
C32A0.6894 (2)0.65118 (16)0.13376 (10)0.0346 (6)
H32A0.6211720.6533140.1327000.042*
C33A0.38131 (16)0.93432 (13)0.10943 (8)0.0201 (5)
C34A0.32784 (17)1.00600 (13)0.12636 (8)0.0222 (5)
C35A0.2296 (2)1.01144 (17)0.12761 (11)0.0402 (7)
H35A0.1945930.9681970.1175790.048*
C36A0.1810 (2)1.07999 (18)0.14348 (12)0.0439 (7)
H36A0.1129021.0833760.1443130.053*
C37A0.2308 (2)1.14256 (15)0.15792 (10)0.0342 (6)
H37A0.1974201.1895150.1684510.041*
C38A0.3289 (2)1.13745 (16)0.15717 (13)0.0452 (8)
H38A0.3634461.1808790.1673240.054*
C39A0.3782 (2)1.06897 (15)0.14161 (12)0.0383 (7)
H39A0.4461641.0653620.1414300.046*
C40A0.85429 (17)0.67146 (15)0.06976 (9)0.0258 (5)
C41A0.85979 (17)0.58503 (15)0.07928 (9)0.0268 (5)
C42A0.94231 (19)0.54378 (17)0.05985 (10)0.0349 (6)
H42A0.9946100.5716910.0397650.042*
C43A0.9483 (2)0.46300 (18)0.06963 (11)0.0394 (7)
H43A1.0051770.4353650.0565900.047*
C44A0.8722 (2)0.42134 (17)0.09833 (10)0.0360 (6)
H44A0.8766920.3652940.1047410.043*
C45A0.78982 (19)0.46150 (16)0.11761 (10)0.0341 (6)
H45A0.7373390.4332060.1372900.041*
C46A0.78399 (18)0.54318 (16)0.10813 (10)0.0315 (6)
H46A0.7273930.5708110.1215600.038*
C47A0.76743 (19)0.96858 (16)0.06143 (11)0.0370 (6)
H47D0.7724080.9657000.0968910.056*
H47E0.7682831.0246530.0491770.056*
H47F0.8223300.9407220.0432160.056*
C48A0.6656 (2)0.93651 (16)0.00038 (10)0.0358 (6)
H48D0.7165340.9052550.0184100.054*
H48E0.6717550.9926240.0118020.054*
H48F0.6019330.9158200.0039190.054*
C49A0.7266 (2)0.83834 (19)0.18419 (11)0.0434 (7)
H49D0.7341860.7926350.2071850.065*
H49E0.7230580.8876260.2021010.065*
H49F0.7823280.8413790.1574880.065*
C50A0.5533 (2)0.82403 (17)0.20201 (10)0.0367 (6)
H50D0.4947600.8153810.1872300.055*
H50E0.5475710.8741610.2190720.055*
H50F0.5610240.7795940.2258810.055*
Cl10.9285 (3)1.1746 (2)0.11598 (13)0.0669 (10)0.357 (2)
Cl21.0097 (3)1.0617 (2)0.04681 (14)0.0539 (9)0.357 (2)
C25S1.0205 (7)1.1567 (6)0.0675 (4)0.046 (2)0.357 (2)
H25B1.0177041.1968370.0397940.056*0.357 (2)
H25C1.0841101.1622640.0788170.056*0.357 (2)
Cl31.0223 (2)0.79436 (19)0.14804 (13)0.0590 (9)0.406 (2)
Cl41.0338 (3)0.8803 (3)0.23589 (13)0.0950 (15)0.406 (2)
C26S1.0943 (6)0.8270 (7)0.1895 (4)0.066 (3)0.406 (2)
H26A1.1239510.7798860.2046100.079*0.406 (2)
H26B1.1474940.8605590.1709730.079*0.406 (2)
C1S0.0684 (2)0.09231 (18)0.39313 (12)0.0429 (7)
H1S0.0861580.1467290.3971410.052*
C2S0.0093 (2)0.05709 (19)0.43123 (11)0.0407 (7)
H2S0.0140960.0872790.4611190.049*
C3S0.0151 (2)0.02124 (19)0.42557 (12)0.0435 (7)
H3S0.0552990.0458570.4516850.052*
C4S0.0184 (2)0.06485 (19)0.38206 (15)0.0526 (9)
H4S0.0018580.1195810.3782830.063*
C5S0.0759 (2)0.0288 (2)0.34410 (12)0.0540 (9)
H5S0.0979300.0584580.3138190.065*
C6S0.1015 (2)0.0497 (2)0.34990 (12)0.0480 (8)
H6S0.1420550.0743670.3239140.058*
C7S0.9702 (4)1.1481 (2)0.07599 (17)0.0587 (17)0.643 (2)
H7S0.9802921.1962890.0558970.070*0.643 (2)
C8S1.0034 (3)1.0762 (3)0.05692 (12)0.064 (3)0.643 (2)
H8S1.0361851.0752260.0237920.077*0.643 (2)
C9S0.9886 (3)1.0056 (2)0.08633 (14)0.0489 (12)0.643 (2)
H9S1.0112900.9564720.0732940.059*0.643 (2)
C10S0.9406 (2)1.0070 (2)0.13480 (13)0.0542 (13)0.643 (2)
H10S0.9305020.9587790.1549010.065*0.643 (2)
C11S0.9074 (3)1.0789 (3)0.15388 (12)0.0531 (13)0.643 (2)
H11S0.8746101.0798420.1870070.064*0.643 (2)
C12S0.9222 (3)1.1494 (2)0.12447 (18)0.070 (3)0.643 (2)
H12S0.8995031.1985970.1375060.083*0.643 (2)
C13S0.9655 (5)0.9447 (3)0.21569 (18)0.0416 (19)0.357 (2)
H13S0.9419960.9872810.2356800.050*0.357 (2)
C14S0.9531 (4)0.9463 (3)0.16610 (19)0.0399 (19)0.357 (2)
H14S0.9210880.9900280.1522080.048*0.357 (2)
C15S0.9876 (4)0.8840 (3)0.13685 (16)0.0382 (19)0.357 (2)
H15S0.9790830.8851190.1029580.046*0.357 (2)
C16S1.0344 (5)0.8201 (3)0.1572 (2)0.052 (4)0.357 (2)
H16S1.0579850.7774620.1371800.063*0.357 (2)
C17S1.0469 (5)0.8184 (3)0.2068 (2)0.039 (2)0.357 (2)
H17S1.0788940.7747130.2206520.047*0.357 (2)
C18S1.0124 (6)0.8807 (4)0.23601 (17)0.039 (3)0.357 (2)
H18S1.0209000.8796220.2699030.047*0.357 (2)
C19S0.9980 (10)0.8603 (8)0.2339 (4)0.071 (2)*0.237 (2)
H19S0.9833260.8884210.2634310.085*0.237 (2)
C20S1.0894 (9)0.8676 (8)0.2055 (5)0.071 (2)*0.237 (2)
H20S1.1372410.9006860.2155880.085*0.237 (2)
C21S1.1109 (7)0.8265 (9)0.1624 (5)0.071 (2)*0.237 (2)
H21S1.1733410.8314600.1429460.085*0.237 (2)
C22S1.0409 (10)0.7781 (9)0.1476 (4)0.071 (2)*0.237 (2)
H22S1.0555260.7499700.1181450.085*0.237 (2)
C23S0.9494 (8)0.7708 (7)0.1761 (5)0.071 (2)*0.237 (2)
H23S0.9016120.7377040.1659880.085*0.237 (2)
C24S0.9280 (7)0.8119 (8)0.2192 (4)0.071 (2)*0.237 (2)
H24S0.8655100.8069290.2386310.085*0.237 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.01761 (11)0.01427 (11)0.01456 (11)0.00046 (8)0.00293 (8)0.00102 (8)
Zr20.01791 (11)0.01568 (11)0.01906 (12)0.00183 (8)0.00321 (8)0.00110 (8)
N10.0238 (10)0.0195 (10)0.0190 (10)0.0019 (8)0.0030 (8)0.0000 (8)
N20.0199 (9)0.0197 (10)0.0179 (10)0.0003 (7)0.0030 (7)0.0005 (7)
N30.0271 (10)0.0204 (10)0.0226 (11)0.0037 (8)0.0047 (8)0.0026 (8)
N40.0306 (11)0.0203 (10)0.0234 (11)0.0033 (8)0.0059 (8)0.0032 (8)
N50.0228 (10)0.0252 (11)0.0199 (10)0.0013 (8)0.0010 (8)0.0004 (8)
N60.0209 (10)0.0221 (10)0.0171 (10)0.0006 (8)0.0037 (7)0.0020 (8)
N70.0252 (10)0.0311 (11)0.0166 (10)0.0003 (8)0.0045 (8)0.0024 (8)
N80.0253 (11)0.0384 (12)0.0199 (11)0.0036 (9)0.0009 (8)0.0055 (9)
N90.0238 (10)0.0169 (10)0.0230 (10)0.0004 (8)0.0052 (8)0.0024 (8)
N100.0220 (10)0.0206 (10)0.0176 (10)0.0018 (8)0.0032 (8)0.0006 (8)
N110.0209 (10)0.0243 (10)0.0193 (10)0.0012 (8)0.0009 (8)0.0033 (8)
N120.0214 (10)0.0191 (10)0.0177 (10)0.0017 (7)0.0034 (7)0.0005 (7)
N130.0249 (10)0.0195 (10)0.0193 (10)0.0010 (8)0.0012 (8)0.0012 (8)
N140.0231 (10)0.0234 (10)0.0219 (11)0.0024 (8)0.0018 (8)0.0008 (8)
N150.0201 (9)0.0160 (9)0.0185 (10)0.0004 (7)0.0019 (7)0.0008 (7)
N160.0194 (9)0.0151 (9)0.0173 (9)0.0002 (7)0.0019 (7)0.0009 (7)
N170.0189 (9)0.0159 (9)0.0186 (10)0.0006 (7)0.0033 (7)0.0021 (7)
N180.0213 (10)0.0182 (10)0.0172 (10)0.0002 (7)0.0028 (7)0.0024 (7)
N190.0231 (10)0.0197 (10)0.0202 (10)0.0026 (8)0.0057 (8)0.0028 (8)
N200.0213 (10)0.0186 (10)0.0180 (10)0.0010 (7)0.0048 (7)0.0002 (7)
N210.0220 (10)0.0158 (9)0.0184 (10)0.0023 (7)0.0034 (7)0.0010 (7)
N220.0244 (10)0.0153 (9)0.0213 (10)0.0002 (7)0.0041 (8)0.0023 (7)
N230.0211 (10)0.0199 (10)0.0226 (10)0.0024 (8)0.0048 (8)0.0009 (8)
N240.0228 (10)0.0206 (10)0.0261 (11)0.0040 (8)0.0043 (8)0.0012 (8)
N250.0231 (11)0.0275 (11)0.0336 (12)0.0024 (8)0.0004 (9)0.0010 (9)
N260.0226 (10)0.0284 (12)0.0370 (13)0.0009 (9)0.0017 (9)0.0009 (9)
N270.0215 (10)0.0183 (10)0.0230 (11)0.0019 (8)0.0036 (8)0.0012 (8)
N280.0267 (10)0.0179 (10)0.0236 (11)0.0020 (8)0.0058 (8)0.0004 (8)
C10.0190 (11)0.0207 (12)0.0210 (12)0.0021 (9)0.0017 (9)0.0018 (9)
C20.0266 (12)0.0251 (12)0.0207 (12)0.0055 (10)0.0012 (9)0.0002 (10)
C30.0389 (15)0.0270 (13)0.0228 (13)0.0072 (11)0.0062 (11)0.0012 (10)
C40.0501 (17)0.0375 (16)0.0241 (14)0.0139 (13)0.0109 (12)0.0112 (11)
C50.0525 (18)0.0486 (18)0.0172 (13)0.0188 (14)0.0050 (12)0.0013 (12)
C60.0491 (17)0.0377 (16)0.0266 (15)0.0101 (13)0.0018 (12)0.0093 (12)
C70.0343 (14)0.0287 (14)0.0246 (13)0.0018 (11)0.0013 (10)0.0054 (10)
C80.0267 (12)0.0271 (13)0.0168 (12)0.0002 (10)0.0030 (9)0.0006 (9)
C90.0286 (13)0.0310 (14)0.0193 (12)0.0047 (10)0.0016 (10)0.0000 (10)
C100.0303 (14)0.062 (2)0.0260 (14)0.0050 (13)0.0055 (11)0.0115 (13)
C110.0390 (16)0.077 (2)0.0253 (15)0.0158 (15)0.0040 (12)0.0189 (15)
C120.0308 (14)0.068 (2)0.0244 (14)0.0133 (14)0.0003 (11)0.0034 (13)
C130.0301 (14)0.0504 (18)0.0296 (15)0.0027 (12)0.0047 (11)0.0001 (13)
C140.0324 (14)0.0317 (14)0.0265 (14)0.0002 (11)0.0046 (11)0.0010 (11)
C150.0273 (12)0.0222 (12)0.0273 (13)0.0009 (10)0.0055 (10)0.0067 (10)
C160.0398 (15)0.0215 (13)0.0374 (15)0.0085 (11)0.0144 (12)0.0031 (11)
C170.0218 (12)0.0229 (12)0.0288 (13)0.0036 (9)0.0076 (10)0.0041 (10)
C180.0221 (12)0.0247 (12)0.0230 (12)0.0010 (9)0.0052 (9)0.0039 (9)
C190.0231 (12)0.0199 (12)0.0230 (12)0.0011 (9)0.0019 (9)0.0017 (9)
C200.0242 (12)0.0256 (13)0.0299 (14)0.0046 (10)0.0036 (10)0.0037 (10)
C210.0390 (16)0.0505 (19)0.0416 (18)0.0133 (14)0.0116 (13)0.0213 (14)
C220.059 (2)0.064 (2)0.046 (2)0.0138 (17)0.0161 (16)0.0310 (17)
C230.0473 (19)0.0483 (19)0.055 (2)0.0007 (15)0.0262 (16)0.0159 (16)
C240.0222 (14)0.056 (2)0.056 (2)0.0024 (13)0.0082 (13)0.0007 (16)
C250.0299 (14)0.0440 (17)0.0373 (16)0.0011 (12)0.0000 (12)0.0033 (13)
C260.0200 (11)0.0180 (11)0.0163 (11)0.0015 (9)0.0001 (8)0.0004 (9)
C270.0181 (11)0.0205 (11)0.0183 (12)0.0020 (9)0.0004 (9)0.0016 (9)
C280.0221 (12)0.0218 (12)0.0224 (12)0.0006 (9)0.0026 (9)0.0001 (9)
C290.0247 (12)0.0292 (13)0.0232 (13)0.0021 (10)0.0044 (10)0.0021 (10)
C300.0304 (13)0.0245 (13)0.0247 (13)0.0059 (10)0.0003 (10)0.0066 (10)
C310.0331 (13)0.0168 (12)0.0273 (13)0.0015 (10)0.0017 (10)0.0002 (10)
C320.0232 (12)0.0220 (12)0.0196 (12)0.0019 (9)0.0012 (9)0.0005 (9)
C330.0225 (11)0.0170 (11)0.0160 (11)0.0004 (9)0.0045 (9)0.0002 (8)
C340.0270 (12)0.0215 (12)0.0200 (12)0.0061 (9)0.0067 (9)0.0026 (9)
C350.0280 (14)0.0404 (16)0.0558 (19)0.0068 (12)0.0143 (13)0.0271 (14)
C360.0302 (16)0.064 (2)0.082 (3)0.0179 (15)0.0168 (16)0.0430 (19)
C370.0458 (18)0.0438 (18)0.069 (2)0.0206 (14)0.0223 (16)0.0329 (16)
C380.0453 (17)0.0255 (14)0.0466 (18)0.0060 (12)0.0143 (13)0.0144 (12)
C390.0327 (14)0.0235 (13)0.0328 (14)0.0035 (10)0.0071 (11)0.0059 (10)
C400.0210 (11)0.0256 (12)0.0211 (12)0.0004 (9)0.0028 (9)0.0044 (9)
C410.0246 (12)0.0253 (12)0.0213 (12)0.0009 (9)0.0057 (9)0.0046 (9)
C420.0289 (14)0.0333 (15)0.0379 (16)0.0045 (11)0.0036 (11)0.0028 (12)
C430.0333 (15)0.0363 (16)0.0451 (17)0.0135 (12)0.0023 (12)0.0080 (13)
C440.0429 (15)0.0240 (13)0.0295 (14)0.0064 (11)0.0123 (11)0.0059 (10)
C450.0319 (13)0.0263 (13)0.0288 (14)0.0009 (10)0.0097 (11)0.0008 (10)
C460.0216 (12)0.0284 (13)0.0264 (13)0.0016 (10)0.0050 (10)0.0015 (10)
C470.0257 (13)0.0202 (13)0.0556 (18)0.0052 (10)0.0094 (12)0.0073 (12)
C480.0484 (16)0.0225 (13)0.0221 (13)0.0022 (11)0.0069 (11)0.0045 (10)
C490.0321 (15)0.0516 (18)0.0414 (17)0.0023 (13)0.0129 (12)0.0205 (14)
C500.0365 (14)0.0312 (14)0.0238 (13)0.0066 (11)0.0003 (11)0.0001 (10)
Zr1A0.01933 (11)0.01475 (11)0.01675 (12)0.00050 (8)0.00290 (8)0.00006 (8)
Zr2A0.01831 (11)0.01878 (12)0.02023 (12)0.00096 (8)0.00181 (8)0.00063 (8)
N1A0.0230 (10)0.0208 (10)0.0223 (11)0.0006 (8)0.0028 (8)0.0013 (8)
N2A0.0230 (10)0.0193 (10)0.0228 (11)0.0008 (8)0.0034 (8)0.0001 (8)
N3A0.0310 (11)0.0209 (10)0.0190 (10)0.0033 (8)0.0033 (8)0.0024 (8)
N4A0.0341 (11)0.0216 (10)0.0202 (10)0.0023 (8)0.0050 (8)0.0025 (8)
N5A0.0251 (10)0.0242 (10)0.0208 (11)0.0012 (8)0.0021 (8)0.0013 (8)
N6A0.0239 (10)0.0213 (10)0.0195 (10)0.0006 (8)0.0037 (8)0.0008 (8)
N7A0.0269 (11)0.0290 (11)0.0199 (11)0.0036 (8)0.0053 (8)0.0000 (8)
N8A0.0275 (11)0.0275 (11)0.0203 (11)0.0016 (8)0.0036 (8)0.0006 (8)
N9A0.0261 (11)0.0213 (10)0.0360 (12)0.0017 (8)0.0102 (9)0.0048 (9)
N10A0.0243 (10)0.0257 (11)0.0183 (10)0.0004 (8)0.0025 (8)0.0034 (8)
N11A0.0248 (10)0.0194 (10)0.0244 (11)0.0002 (8)0.0041 (8)0.0029 (8)
N12A0.0221 (10)0.0172 (9)0.0226 (10)0.0000 (8)0.0034 (8)0.0011 (8)
N13A0.0215 (10)0.0206 (10)0.0189 (10)0.0014 (8)0.0030 (8)0.0024 (8)
N14A0.0226 (10)0.0203 (10)0.0221 (10)0.0018 (8)0.0034 (8)0.0034 (8)
N15A0.0261 (10)0.0221 (10)0.0206 (11)0.0004 (8)0.0023 (8)0.0018 (8)
N16A0.0242 (10)0.0193 (10)0.0181 (10)0.0008 (8)0.0020 (8)0.0010 (8)
N17A0.0235 (10)0.0224 (10)0.0205 (10)0.0013 (8)0.0001 (8)0.0004 (8)
N18A0.0253 (10)0.0240 (10)0.0210 (10)0.0015 (8)0.0005 (8)0.0006 (8)
N19A0.0233 (10)0.0215 (10)0.0199 (10)0.0040 (8)0.0034 (8)0.0011 (8)
N20A0.0206 (9)0.0197 (10)0.0191 (10)0.0009 (8)0.0031 (7)0.0000 (8)
N21A0.0237 (10)0.0162 (9)0.0184 (10)0.0011 (7)0.0013 (8)0.0010 (7)
N22A0.0247 (10)0.0162 (10)0.0221 (10)0.0003 (8)0.0013 (8)0.0004 (8)
N23A0.0218 (10)0.0273 (11)0.0217 (10)0.0002 (8)0.0047 (8)0.0024 (8)
N24A0.0230 (10)0.0272 (11)0.0255 (11)0.0025 (8)0.0037 (8)0.0010 (8)
N25A0.0219 (11)0.0398 (13)0.0361 (13)0.0011 (9)0.0028 (9)0.0003 (10)
N26A0.0264 (11)0.0380 (13)0.0398 (14)0.0035 (10)0.0010 (10)0.0021 (10)
N27A0.0254 (11)0.0210 (10)0.0251 (11)0.0028 (8)0.0018 (8)0.0009 (8)
N28A0.0351 (12)0.0259 (11)0.0222 (11)0.0014 (9)0.0009 (9)0.0008 (8)
C1A0.0193 (11)0.0208 (12)0.0198 (12)0.0008 (9)0.0006 (9)0.0001 (9)
C21A0.0334 (14)0.0254 (13)0.0323 (14)0.0003 (10)0.0106 (11)0.0031 (11)
C2A0.0247 (12)0.0291 (13)0.0185 (12)0.0017 (10)0.0009 (9)0.0029 (10)
C3A0.0326 (14)0.0317 (14)0.0269 (14)0.0015 (11)0.0051 (11)0.0056 (11)
C4A0.0403 (16)0.0453 (17)0.0271 (15)0.0043 (13)0.0079 (12)0.0149 (12)
C5A0.0455 (17)0.061 (2)0.0195 (14)0.0090 (14)0.0066 (12)0.0062 (13)
C6A0.0524 (18)0.0445 (17)0.0233 (14)0.0025 (14)0.0034 (12)0.0061 (12)
C7A0.0385 (15)0.0324 (14)0.0221 (13)0.0022 (11)0.0040 (11)0.0006 (10)
C8A0.0261 (12)0.0195 (11)0.0188 (12)0.0026 (9)0.0025 (9)0.0009 (9)
C9A0.0276 (12)0.0204 (12)0.0205 (12)0.0003 (9)0.0004 (9)0.0035 (9)
C10A0.0295 (13)0.0290 (13)0.0222 (13)0.0020 (10)0.0020 (10)0.0022 (10)
C11A0.0387 (15)0.0291 (14)0.0221 (13)0.0030 (11)0.0012 (11)0.0011 (10)
C12A0.0374 (15)0.0314 (14)0.0307 (15)0.0107 (11)0.0041 (11)0.0046 (11)
C13A0.0337 (15)0.0410 (16)0.0345 (16)0.0110 (12)0.0048 (12)0.0074 (12)
C14A0.0374 (14)0.0344 (14)0.0222 (13)0.0081 (11)0.0067 (11)0.0011 (11)
C15A0.0333 (14)0.0194 (12)0.0409 (16)0.0009 (10)0.0082 (11)0.0026 (11)
C16A0.0327 (14)0.0274 (14)0.0397 (16)0.0044 (11)0.0105 (12)0.0008 (11)
C17A0.0265 (13)0.0297 (14)0.0344 (15)0.0069 (10)0.0106 (11)0.0084 (11)
C18A0.0228 (12)0.0250 (13)0.0340 (14)0.0027 (10)0.0062 (10)0.0030 (10)
C19A0.0215 (11)0.0220 (12)0.0211 (12)0.0025 (9)0.0019 (9)0.0010 (9)
C20A0.0227 (12)0.0230 (12)0.0251 (13)0.0030 (9)0.0017 (9)0.0035 (10)
C22A0.0415 (16)0.0236 (13)0.0441 (17)0.0009 (11)0.0124 (13)0.0040 (12)
C23A0.0391 (15)0.0282 (14)0.0322 (15)0.0084 (11)0.0065 (11)0.0094 (11)
C24A0.0304 (13)0.0350 (14)0.0249 (13)0.0061 (11)0.0063 (10)0.0030 (11)
C25A0.0269 (12)0.0253 (13)0.0235 (13)0.0032 (10)0.0028 (10)0.0011 (10)
C26A0.0264 (12)0.0169 (11)0.0208 (12)0.0012 (9)0.0014 (9)0.0009 (9)
C27A0.0327 (13)0.0196 (12)0.0241 (13)0.0036 (10)0.0023 (10)0.0000 (10)
C28A0.0340 (15)0.0561 (19)0.0262 (14)0.0110 (13)0.0040 (11)0.0015 (13)
C29A0.0386 (17)0.068 (2)0.0385 (18)0.0253 (15)0.0031 (13)0.0069 (15)
C30A0.067 (2)0.0395 (17)0.0324 (17)0.0182 (15)0.0127 (15)0.0022 (13)
C31A0.062 (2)0.0388 (17)0.0293 (16)0.0066 (14)0.0055 (14)0.0111 (12)
C32A0.0424 (16)0.0304 (14)0.0293 (15)0.0091 (12)0.0031 (12)0.0091 (11)
C33A0.0252 (12)0.0190 (11)0.0151 (11)0.0007 (9)0.0009 (9)0.0018 (9)
C34A0.0293 (12)0.0196 (12)0.0163 (12)0.0043 (9)0.0004 (9)0.0011 (9)
C35A0.0363 (15)0.0374 (16)0.0528 (19)0.0117 (12)0.0179 (13)0.0224 (14)
C36A0.0355 (16)0.0447 (18)0.056 (2)0.0209 (13)0.0160 (14)0.0208 (15)
C37A0.0465 (16)0.0230 (13)0.0298 (14)0.0116 (11)0.0046 (12)0.0012 (11)
C38A0.0422 (17)0.0196 (14)0.070 (2)0.0014 (12)0.0068 (15)0.0105 (13)
C39A0.0274 (14)0.0234 (14)0.061 (2)0.0012 (11)0.0053 (13)0.0091 (13)
C40A0.0197 (12)0.0338 (14)0.0247 (13)0.0040 (10)0.0045 (9)0.0050 (10)
C41A0.0253 (12)0.0331 (14)0.0239 (13)0.0057 (10)0.0079 (10)0.0065 (10)
C42A0.0314 (14)0.0413 (16)0.0315 (15)0.0109 (12)0.0023 (11)0.0063 (12)
C43A0.0370 (15)0.0473 (18)0.0342 (16)0.0177 (13)0.0040 (12)0.0093 (13)
C44A0.0453 (16)0.0329 (15)0.0346 (15)0.0105 (12)0.0181 (13)0.0108 (12)
C45A0.0328 (14)0.0328 (15)0.0386 (16)0.0030 (11)0.0111 (12)0.0039 (12)
C46A0.0279 (13)0.0332 (14)0.0340 (15)0.0083 (11)0.0053 (11)0.0058 (11)
C47A0.0282 (14)0.0276 (14)0.0529 (18)0.0076 (11)0.0006 (12)0.0003 (12)
C48A0.0554 (18)0.0248 (13)0.0247 (14)0.0030 (12)0.0014 (12)0.0016 (10)
C49A0.0457 (17)0.0542 (19)0.0311 (16)0.0053 (14)0.0043 (13)0.0134 (13)
C50A0.0453 (16)0.0364 (15)0.0255 (14)0.0032 (12)0.0039 (12)0.0021 (11)
Cl10.077 (2)0.0678 (19)0.0477 (17)0.0210 (15)0.0134 (15)0.0055 (15)
Cl20.061 (2)0.0524 (16)0.0445 (15)0.0176 (14)0.0021 (13)0.0008 (13)
C25S0.048 (6)0.051 (6)0.040 (5)0.011 (5)0.010 (5)0.002 (4)
Cl30.0656 (19)0.0556 (18)0.0608 (16)0.0213 (14)0.0219 (13)0.0144 (14)
Cl40.077 (2)0.157 (4)0.057 (2)0.022 (2)0.0135 (16)0.049 (2)
C26S0.044 (6)0.079 (8)0.078 (8)0.021 (5)0.008 (5)0.035 (7)
C1S0.0385 (16)0.0365 (16)0.058 (2)0.0031 (13)0.0189 (14)0.0094 (14)
C2S0.0341 (15)0.0507 (19)0.0380 (17)0.0108 (13)0.0093 (12)0.0028 (14)
C3S0.0302 (15)0.055 (2)0.0495 (19)0.0025 (13)0.0126 (13)0.0191 (15)
C4S0.0496 (19)0.0336 (17)0.084 (3)0.0050 (14)0.0389 (19)0.0006 (17)
C5S0.0379 (17)0.082 (3)0.0431 (19)0.0263 (17)0.0168 (14)0.0194 (18)
C6S0.0308 (15)0.075 (2)0.0408 (18)0.0004 (15)0.0075 (13)0.0202 (17)
C7S0.042 (3)0.068 (4)0.070 (4)0.005 (3)0.027 (3)0.010 (3)
C8S0.049 (5)0.083 (5)0.066 (5)0.007 (4)0.029 (4)0.008 (4)
C9S0.039 (3)0.054 (3)0.059 (3)0.001 (2)0.022 (2)0.016 (2)
C10S0.043 (3)0.062 (3)0.061 (3)0.014 (2)0.022 (2)0.006 (2)
C11S0.033 (2)0.081 (3)0.045 (3)0.005 (2)0.000 (2)0.012 (2)
C12S0.028 (3)0.096 (6)0.085 (5)0.005 (3)0.011 (3)0.005 (4)
C13S0.050 (4)0.033 (3)0.039 (4)0.005 (3)0.003 (3)0.000 (3)
C14S0.034 (4)0.040 (5)0.044 (5)0.005 (3)0.002 (3)0.005 (4)
C15S0.041 (4)0.042 (5)0.030 (4)0.013 (4)0.003 (3)0.000 (3)
C16S0.050 (7)0.048 (8)0.054 (9)0.008 (6)0.007 (6)0.005 (6)
C17S0.046 (5)0.034 (4)0.037 (5)0.008 (3)0.001 (4)0.002 (3)
C18S0.060 (6)0.031 (4)0.023 (5)0.010 (4)0.002 (4)0.000 (3)
Geometric parameters (Å, º) top
Zr1—N22.2935 (18)N10A—C18A1.479 (3)
Zr1—N62.3340 (19)N11A—N12A1.327 (3)
Zr1—N91.9798 (19)N11A—C19A1.343 (3)
Zr1—N102.4073 (19)N12A—N13A1.325 (3)
Zr1—N122.3829 (18)N13A—N14A1.335 (3)
Zr1—N162.3741 (18)N14A—C19A1.332 (3)
Zr1—N202.3699 (19)N15A—N16A1.326 (3)
Zr2—N132.3115 (19)N15A—C26A1.337 (3)
Zr2—N172.3085 (17)N16A—N17A1.319 (3)
Zr2—N212.3227 (18)N17A—N18A1.331 (3)
Zr2—N232.3027 (19)N18A—C26A1.336 (3)
Zr2—N242.2238 (19)N19A—N20A1.324 (3)
Zr2—N272.3218 (19)N19A—C33A1.337 (3)
Zr2—N281.975 (2)N20A—N21A1.324 (3)
N1—N21.343 (3)N21A—N22A1.333 (3)
N1—C11.332 (3)N22A—C33A1.332 (3)
N2—N31.328 (3)N23A—N24A1.350 (3)
N3—N41.328 (3)N23A—C40A1.338 (3)
N4—C11.343 (3)N24A—N25A1.305 (3)
N5—N61.341 (3)N25A—N26A1.332 (3)
N5—C81.327 (3)N26A—C40A1.347 (3)
N6—N71.333 (3)N27A—H27A0.849 (16)
N7—N81.317 (3)N27A—C47A1.485 (3)
N8—C81.347 (3)N27A—C48A1.486 (3)
N9—C151.463 (3)N28A—C49A1.461 (3)
N9—C161.449 (3)N28A—C50A1.461 (3)
N10—H100.847 (16)C1A—C2A1.472 (3)
N10—C171.484 (3)C21A—H21A0.9500
N10—C181.474 (3)C21A—C20A1.386 (3)
N11—N121.328 (3)C21A—C22A1.382 (3)
N11—C191.341 (3)C2A—C3A1.388 (3)
N12—N131.316 (3)C2A—C7A1.394 (3)
N13—N141.328 (3)C3A—H3A0.9500
N14—C191.336 (3)C3A—C4A1.381 (4)
N15—N161.332 (2)C4A—H4A0.9500
N15—C261.342 (3)C4A—C5A1.376 (4)
N16—N171.325 (2)C5A—H5A0.9500
N17—N181.326 (2)C5A—C6A1.377 (4)
N18—C261.335 (3)C6A—H6A0.9500
N19—N201.325 (3)C6A—C7A1.393 (4)
N19—C331.338 (3)C7A—H7A0.9500
N20—N211.325 (2)C8A—C9A1.470 (3)
N21—N221.336 (3)C9A—C10A1.389 (3)
N22—C331.333 (3)C9A—C14A1.391 (3)
N23—N241.349 (3)C10A—H10C0.9500
N23—C401.338 (3)C10A—C11A1.384 (3)
N24—N251.307 (3)C11A—H11A0.9500
N25—N261.331 (3)C11A—C12A1.379 (4)
N26—C401.348 (3)C12A—H12A0.9500
N27—H270.843 (16)C12A—C13A1.375 (4)
N27—C471.485 (3)C13A—H13A0.9500
N27—C481.484 (3)C13A—C14A1.390 (4)
N28—C491.457 (3)C14A—H14A0.9500
N28—C501.463 (3)C15A—H15D0.9800
C1—C21.469 (3)C15A—H15E0.9800
C2—C31.386 (4)C15A—H15F0.9800
C2—C71.394 (3)C16A—H16D0.9800
C3—H30.9500C16A—H16E0.9800
C3—C41.387 (4)C16A—H16F0.9800
C4—H40.9500C17A—H17D0.9800
C4—C51.385 (4)C17A—H17E0.9800
C5—H50.9500C17A—H17F0.9800
C5—C61.374 (4)C18A—H18D0.9800
C6—H60.9500C18A—H18E0.9800
C6—C71.387 (4)C18A—H18F0.9800
C7—H70.9500C19A—C20A1.467 (3)
C8—C91.459 (3)C20A—C25A1.389 (3)
C9—C101.392 (4)C22A—H22A0.9500
C9—C141.389 (3)C22A—C23A1.385 (4)
C10—H10A0.9500C23A—H23A0.9500
C10—C111.380 (4)C23A—C24A1.379 (4)
C11—H110.9500C24A—H24A0.9500
C11—C121.377 (4)C24A—C25A1.389 (3)
C12—H120.9500C25A—H25A0.9500
C12—C131.384 (4)C26A—C27A1.466 (3)
C13—H130.9500C27A—C28A1.380 (4)
C13—C141.379 (4)C27A—C32A1.386 (4)
C14—H140.9500C28A—H28A0.9500
C15—H15A0.9800C28A—C29A1.384 (4)
C15—H15B0.9800C29A—H29A0.9500
C15—H15C0.9800C29A—C30A1.374 (5)
C16—H16A0.9800C30A—H30A0.9500
C16—H16B0.9800C30A—C31A1.378 (5)
C16—H16C0.9800C31A—H31A0.9500
C17—H17A0.9800C31A—C32A1.383 (4)
C17—H17B0.9800C32A—H32A0.9500
C17—H17C0.9800C33A—C34A1.472 (3)
C18—H18A0.9800C34A—C35A1.370 (4)
C18—H18B0.9800C34A—C39A1.386 (4)
C18—H18C0.9800C35A—H35A0.9500
C19—C201.475 (3)C35A—C36A1.390 (4)
C20—C211.384 (4)C36A—H36A0.9500
C20—C251.390 (4)C36A—C37A1.367 (4)
C21—H210.9500C37A—H37A0.9500
C21—C221.389 (4)C37A—C38A1.369 (4)
C22—H220.9500C38A—H38A0.9500
C22—C231.365 (5)C38A—C39A1.391 (4)
C23—H230.9500C39A—H39A0.9500
C23—C241.382 (5)C40A—C41A1.462 (4)
C24—H240.9500C41A—C42A1.392 (3)
C24—C251.381 (4)C41A—C46A1.385 (4)
C25—H250.9500C42A—H42A0.9500
C26—C271.464 (3)C42A—C43A1.371 (4)
C27—C281.396 (3)C43A—H43A0.9500
C27—C321.391 (3)C43A—C44A1.384 (4)
C28—H280.9500C44A—H44A0.9500
C28—C291.381 (3)C44A—C45A1.380 (4)
C29—H290.9500C45A—H45A0.9500
C29—C301.382 (3)C45A—C46A1.384 (4)
C30—H300.9500C46A—H46A0.9500
C30—C311.386 (3)C47A—H47D0.9800
C31—H310.9500C47A—H47E0.9800
C31—C321.381 (3)C47A—H47F0.9800
C32—H320.9500C48A—H48D0.9800
C33—C341.470 (3)C48A—H48E0.9800
C34—C351.379 (4)C48A—H48F0.9800
C34—C391.386 (3)C49A—H49D0.9800
C35—H350.9500C49A—H49E0.9800
C35—C361.388 (4)C49A—H49F0.9800
C36—H360.9500C50A—H50D0.9800
C36—C371.373 (4)C50A—H50E0.9800
C37—H370.9500C50A—H50F0.9800
C37—C381.368 (4)Cl1—C25S1.736 (11)
C38—H380.9500Cl2—C25S1.732 (11)
C38—C391.384 (4)C25S—H25B0.9900
C39—H390.9500C25S—H25C0.9900
C40—C411.466 (3)Cl3—C26S1.735 (7)
C41—C421.392 (3)Cl4—C26S1.705 (7)
C41—C461.392 (3)C26S—H26A0.9900
C42—H420.9500C26S—H26B0.9900
C42—C431.379 (4)C1S—H1S0.9500
C43—H430.9500C1S—C2S1.383 (4)
C43—C441.377 (4)C1S—C6S1.363 (5)
C44—H440.9500C2S—H2S0.9500
C44—C451.384 (4)C2S—C3S1.363 (4)
C45—H450.9500C3S—H3S0.9500
C45—C461.380 (3)C3S—C4S1.378 (5)
C46—H460.9500C4S—H4S0.9500
C47—H47A0.9800C4S—C5S1.376 (5)
C47—H47B0.9800C5S—H5S0.9500
C47—H47C0.9800C5S—C6S1.372 (5)
C48—H48A0.9800C6S—H6S0.9500
C48—H48B0.9800C7S—H7S0.9500
C48—H48C0.9800C7S—C8S1.3900
C49—H49A0.9800C7S—C12S1.3900
C49—H49B0.9800C8S—H8S0.9500
C49—H49C0.9800C8S—C9S1.3900
C50—H50A0.9800C9S—H9S0.9500
C50—H50B0.9800C9S—C10S1.3900
C50—H50C0.9800C10S—H10S0.9500
Zr1A—N2A2.2856 (19)C10S—C11S1.3900
Zr1A—N6A2.3073 (19)C11S—H11S0.9500
Zr1A—N9A1.987 (2)C11S—C12S1.3900
Zr1A—N10A2.4095 (19)C12S—H12S0.9500
Zr1A—N12A2.3907 (18)C13S—H13S0.9500
Zr1A—N16A2.3651 (19)C13S—C14S1.3900
Zr1A—N20A2.3822 (19)C13S—C18S1.3900
Zr2A—N13A2.2969 (18)C14S—H14S0.9500
Zr2A—N17A2.336 (2)C14S—C15S1.3900
Zr2A—N21A2.3166 (19)C15S—H15S0.9500
Zr2A—N23A2.290 (2)C15S—C16S1.3900
Zr2A—N24A2.214 (2)C16S—H16S0.9500
Zr2A—N27A2.3145 (19)C16S—C17S1.3900
Zr2A—N28A1.989 (2)C17S—H17S0.9500
N1A—N2A1.338 (3)C17S—C18S1.3900
N1A—C1A1.330 (3)C18S—H18S0.9500
N2A—N3A1.325 (3)C19S—H19S0.9500
N3A—N4A1.330 (3)C19S—C20S1.3900
N4A—C1A1.337 (3)C19S—C24S1.3900
N5A—N6A1.347 (3)C20S—H20S0.9500
N5A—C8A1.332 (3)C20S—C21S1.3900
N6A—N7A1.327 (3)C21S—H21S0.9500
N7A—N8A1.323 (3)C21S—C22S1.3900
N8A—C8A1.348 (3)C22S—H22S0.9500
N9A—C15A1.450 (3)C22S—C23S1.3900
N9A—C16A1.466 (3)C23S—H23S0.9500
N10A—H10B0.847 (16)C23S—C24S1.3900
N10A—C17A1.487 (3)C24S—H24S0.9500
N2—Zr1—N6134.97 (7)C1A—N1A—N2A103.40 (18)
N2—Zr1—N1073.39 (6)N1A—N2A—Zr1A123.14 (14)
N2—Zr1—N1270.76 (6)N3A—N2A—Zr1A125.37 (15)
N2—Zr1—N16136.58 (6)N3A—N2A—N1A111.47 (18)
N2—Zr1—N2080.56 (6)N2A—N3A—N4A107.23 (18)
N6—Zr1—N1075.26 (6)N3A—N4A—C1A106.12 (18)
N6—Zr1—N12141.40 (6)C8A—N5A—N6A103.64 (18)
N6—Zr1—N1672.74 (6)N5A—N6A—Zr1A121.77 (14)
N6—Zr1—N2073.79 (6)N7A—N6A—Zr1A126.71 (14)
N9—Zr1—N2119.12 (7)N7A—N6A—N5A110.71 (18)
N9—Zr1—N690.53 (7)N8A—N7A—N6A108.19 (18)
N9—Zr1—N1087.31 (7)N7A—N8A—C8A105.85 (19)
N9—Zr1—N1299.17 (7)C15A—N9A—Zr1A135.77 (17)
N9—Zr1—N1686.27 (7)C15A—N9A—C16A110.9 (2)
N9—Zr1—N20160.32 (7)C16A—N9A—Zr1A113.32 (15)
N12—Zr1—N10141.97 (6)Zr1A—N10A—H10B97.7 (18)
N16—Zr1—N10147.26 (6)C17A—N10A—Zr1A120.15 (14)
N16—Zr1—N1270.77 (6)C17A—N10A—H10B104.6 (18)
N20—Zr1—N1099.73 (6)C18A—N10A—Zr1A114.89 (15)
N20—Zr1—N1286.62 (6)C18A—N10A—H10B109.3 (18)
N20—Zr1—N1677.86 (6)C18A—N10A—C17A108.66 (18)
N13—Zr2—N2179.81 (7)N12A—N11A—C19A104.34 (18)
N13—Zr2—N2794.79 (7)N11A—N12A—Zr1A121.09 (14)
N17—Zr2—N1374.01 (6)N13A—N12A—Zr1A129.15 (14)
N17—Zr2—N2177.41 (6)N13A—N12A—N11A109.39 (17)
N17—Zr2—N27151.53 (6)N12A—N13A—Zr2A135.17 (14)
N23—Zr2—N1389.81 (7)N12A—N13A—N14A110.03 (17)
N23—Zr2—N1788.12 (6)N14A—N13A—Zr2A112.03 (13)
N23—Zr2—N21164.03 (6)C19A—N14A—N13A103.92 (18)
N23—Zr2—N27118.47 (7)N16A—N15A—C26A104.48 (18)
N24—Zr2—N1394.29 (7)N15A—N16A—Zr1A121.02 (14)
N24—Zr2—N17122.35 (7)N17A—N16A—Zr1A129.28 (14)
N24—Zr2—N21157.26 (7)N17A—N16A—N15A109.69 (18)
N24—Zr2—N2334.62 (6)N16A—N17A—Zr2A137.44 (15)
N24—Zr2—N2783.88 (7)N16A—N17A—N18A109.70 (18)
N27—Zr2—N2174.84 (6)N18A—N17A—Zr2A112.34 (14)
N28—Zr2—N13155.40 (7)N17A—N18A—C26A104.23 (18)
N28—Zr2—N1784.68 (7)N20A—N19A—C33A104.74 (18)
N28—Zr2—N2183.74 (7)N19A—N20A—Zr1A116.80 (14)
N28—Zr2—N23101.82 (7)N21A—N20A—Zr1A133.03 (14)
N28—Zr2—N24107.64 (8)N21A—N20A—N19A109.55 (18)
N28—Zr2—N2798.43 (7)N20A—N21A—Zr2A132.39 (14)
C1—N1—N2103.28 (18)N20A—N21A—N22A109.38 (18)
N1—N2—Zr1124.70 (14)N22A—N21A—Zr2A117.53 (14)
N3—N2—Zr1123.62 (14)C33A—N22A—N21A104.56 (18)
N3—N2—N1111.29 (17)N24A—N23A—Zr2A69.52 (12)
N2—N3—N4107.58 (18)C40A—N23A—Zr2A168.90 (17)
N3—N4—C1105.93 (18)C40A—N23A—N24A104.53 (19)
C8—N5—N6104.20 (18)N23A—N24A—Zr2A75.64 (12)
N5—N6—Zr1122.93 (13)N25A—N24A—Zr2A168.83 (17)
N7—N6—Zr1123.18 (14)N25A—N24A—N23A110.8 (2)
N7—N6—N5110.12 (18)N24A—N25A—N26A108.0 (2)
N8—N7—N6108.37 (18)N25A—N26A—C40A106.9 (2)
N7—N8—C8105.84 (19)Zr2A—N27A—H27A108.1 (19)
C15—N9—Zr1105.05 (14)C47A—N27A—Zr2A114.18 (15)
C16—N9—Zr1142.02 (17)C47A—N27A—H27A105.0 (18)
C16—N9—C15112.93 (19)C47A—N27A—C48A109.9 (2)
Zr1—N10—H1095.9 (17)C48A—N27A—Zr2A115.15 (15)
C17—N10—Zr1119.92 (13)C48A—N27A—H27A103.3 (19)
C17—N10—H10105.3 (18)C49A—N28A—Zr2A118.14 (17)
C18—N10—Zr1116.27 (14)C50A—N28A—Zr2A130.06 (18)
C18—N10—H10108.6 (18)C50A—N28A—C49A110.7 (2)
C18—N10—C17108.88 (17)N1A—C1A—N4A111.8 (2)
N12—N11—C19104.57 (18)N1A—C1A—C2A123.8 (2)
N11—N12—Zr1127.83 (14)N4A—C1A—C2A124.4 (2)
N13—N12—Zr1122.40 (14)C20A—C21A—H21A119.9
N13—N12—N11109.37 (17)C22A—C21A—H21A119.9
N12—N13—Zr2143.33 (15)C22A—C21A—C20A120.2 (2)
N12—N13—N14110.20 (18)C3A—C2A—C1A119.8 (2)
N14—N13—Zr2105.68 (13)C3A—C2A—C7A119.4 (2)
N13—N14—C19104.20 (18)C7A—C2A—C1A120.8 (2)
N16—N15—C26104.27 (17)C2A—C3A—H3A119.8
N15—N16—Zr1120.39 (13)C4A—C3A—C2A120.3 (3)
N17—N16—Zr1129.65 (13)C4A—C3A—H3A119.8
N17—N16—N15109.33 (16)C3A—C4A—H4A119.9
N16—N17—Zr2134.22 (13)C5A—C4A—C3A120.2 (3)
N16—N17—N18110.00 (17)C5A—C4A—H4A119.9
N18—N17—Zr2114.01 (13)C4A—C5A—H5A119.9
N17—N18—C26104.36 (17)C4A—C5A—C6A120.2 (3)
N20—N19—C33104.64 (18)C6A—C5A—H5A119.9
N19—N20—Zr1117.06 (13)C5A—C6A—H6A119.9
N21—N20—Zr1133.38 (14)C5A—C6A—C7A120.2 (3)
N21—N20—N19109.53 (17)C7A—C6A—H6A119.9
N20—N21—Zr2131.62 (14)C2A—C7A—H7A120.2
N20—N21—N22109.52 (17)C6A—C7A—C2A119.6 (3)
N22—N21—Zr2117.40 (13)C6A—C7A—H7A120.2
C33—N22—N21104.26 (18)N5A—C8A—N8A111.6 (2)
N24—N23—Zr269.49 (11)N5A—C8A—C9A125.1 (2)
C40—N23—Zr2171.55 (16)N8A—C8A—C9A123.2 (2)
C40—N23—N24104.30 (18)C10A—C9A—C8A120.2 (2)
N23—N24—Zr275.89 (11)C10A—C9A—C14A119.0 (2)
N25—N24—Zr2170.93 (16)C14A—C9A—C8A120.8 (2)
N25—N24—N23111.00 (18)C9A—C10A—H10C119.7
N24—N25—N26107.97 (18)C11A—C10A—C9A120.7 (2)
N25—N26—C40106.70 (19)C11A—C10A—H10C119.7
Zr2—N27—H27105.1 (18)C10A—C11A—H11A120.0
C47—N27—Zr2115.91 (14)C12A—C11A—C10A120.0 (2)
C47—N27—H27106.9 (18)C12A—C11A—H11A120.0
C48—N27—Zr2115.04 (14)C11A—C12A—H12A120.1
C48—N27—H27103.6 (18)C13A—C12A—C11A119.9 (2)
C48—N27—C47109.16 (19)C13A—C12A—H12A120.1
C49—N28—Zr2114.57 (16)C12A—C13A—H13A119.7
C49—N28—C50111.3 (2)C12A—C13A—C14A120.5 (2)
C50—N28—Zr2133.88 (16)C14A—C13A—H13A119.7
N1—C1—N4111.9 (2)C9A—C14A—H14A120.0
N1—C1—C2124.0 (2)C13A—C14A—C9A119.9 (2)
N4—C1—C2124.0 (2)C13A—C14A—H14A120.0
C3—C2—C1119.9 (2)N9A—C15A—H15D109.5
C3—C2—C7119.6 (2)N9A—C15A—H15E109.5
C7—C2—C1120.5 (2)N9A—C15A—H15F109.5
C2—C3—H3119.8H15D—C15A—H15E109.5
C2—C3—C4120.3 (2)H15D—C15A—H15F109.5
C4—C3—H3119.8H15E—C15A—H15F109.5
C3—C4—H4120.2N9A—C16A—H16D109.5
C5—C4—C3119.7 (3)N9A—C16A—H16E109.5
C5—C4—H4120.2N9A—C16A—H16F109.5
C4—C5—H5119.8H16D—C16A—H16E109.5
C6—C5—C4120.4 (2)H16D—C16A—H16F109.5
C6—C5—H5119.8H16E—C16A—H16F109.5
C5—C6—H6119.9N10A—C17A—H17D109.5
C5—C6—C7120.3 (3)N10A—C17A—H17E109.5
C7—C6—H6119.9N10A—C17A—H17F109.5
C2—C7—H7120.1H17D—C17A—H17E109.5
C6—C7—C2119.8 (3)H17D—C17A—H17F109.5
C6—C7—H7120.1H17E—C17A—H17F109.5
N5—C8—N8111.5 (2)N10A—C18A—H18D109.5
N5—C8—C9123.7 (2)N10A—C18A—H18E109.5
N8—C8—C9124.8 (2)N10A—C18A—H18F109.5
C10—C9—C8120.1 (2)H18D—C18A—H18E109.5
C14—C9—C8120.6 (2)H18D—C18A—H18F109.5
C14—C9—C10119.2 (2)H18E—C18A—H18F109.5
C9—C10—H10A119.8N11A—C19A—C20A124.8 (2)
C11—C10—C9120.3 (3)N14A—C19A—N11A112.32 (19)
C11—C10—H10A119.8N14A—C19A—C20A122.8 (2)
C10—C11—H11119.9C21A—C20A—C19A120.0 (2)
C12—C11—C10120.1 (3)C21A—C20A—C25A119.7 (2)
C12—C11—H11119.9C25A—C20A—C19A120.3 (2)
C11—C12—H12120.0C21A—C22A—H22A120.0
C11—C12—C13120.0 (3)C21A—C22A—C23A120.0 (2)
C13—C12—H12120.0C23A—C22A—H22A120.0
C12—C13—H13119.9C22A—C23A—H23A120.0
C14—C13—C12120.2 (3)C24A—C23A—C22A120.1 (2)
C14—C13—H13119.9C24A—C23A—H23A120.0
C9—C14—H14119.9C23A—C24A—H24A120.0
C13—C14—C9120.1 (3)C23A—C24A—C25A120.1 (2)
C13—C14—H14119.9C25A—C24A—H24A120.0
N9—C15—H15A109.5C20A—C25A—C24A119.9 (2)
N9—C15—H15B109.5C20A—C25A—H25A120.1
N9—C15—H15C109.5C24A—C25A—H25A120.1
H15A—C15—H15B109.5N15A—C26A—C27A123.7 (2)
H15A—C15—H15C109.5N18A—C26A—N15A111.9 (2)
H15B—C15—H15C109.5N18A—C26A—C27A124.4 (2)
N9—C16—H16A109.5C28A—C27A—C26A121.5 (2)
N9—C16—H16B109.5C28A—C27A—C32A119.4 (2)
N9—C16—H16C109.5C32A—C27A—C26A119.1 (2)
H16A—C16—H16B109.5C27A—C28A—H28A120.1
H16A—C16—H16C109.5C27A—C28A—C29A119.7 (3)
H16B—C16—H16C109.5C29A—C28A—H28A120.1
N10—C17—H17A109.5C28A—C29A—H29A119.8
N10—C17—H17B109.5C30A—C29A—C28A120.4 (3)
N10—C17—H17C109.5C30A—C29A—H29A119.8
H17A—C17—H17B109.5C29A—C30A—H30A119.8
H17A—C17—H17C109.5C29A—C30A—C31A120.5 (3)
H17B—C17—H17C109.5C31A—C30A—H30A119.8
N10—C18—H18A109.5C30A—C31A—H31A120.4
N10—C18—H18B109.5C30A—C31A—C32A119.1 (3)
N10—C18—H18C109.5C32A—C31A—H31A120.4
H18A—C18—H18B109.5C27A—C32A—H32A119.6
H18A—C18—H18C109.5C31A—C32A—C27A120.8 (3)
H18B—C18—H18C109.5C31A—C32A—H32A119.6
N11—C19—C20125.7 (2)N19A—C33A—C34A124.5 (2)
N14—C19—N11111.6 (2)N22A—C33A—N19A111.8 (2)
N14—C19—C20122.7 (2)N22A—C33A—C34A123.7 (2)
C21—C20—C19120.7 (2)C35A—C34A—C33A121.4 (2)
C21—C20—C25119.5 (2)C35A—C34A—C39A119.5 (2)
C25—C20—C19119.8 (2)C39A—C34A—C33A119.1 (2)
C20—C21—H21119.9C34A—C35A—H35A119.9
C20—C21—C22120.2 (3)C34A—C35A—C36A120.2 (3)
C22—C21—H21119.9C36A—C35A—H35A119.9
C21—C22—H22119.9C35A—C36A—H36A119.8
C23—C22—C21120.2 (3)C37A—C36A—C35A120.3 (3)
C23—C22—H22119.9C37A—C36A—H36A119.8
C22—C23—H23120.1C36A—C37A—H37A120.1
C22—C23—C24119.7 (3)C36A—C37A—C38A119.9 (3)
C24—C23—H23120.1C38A—C37A—H37A120.1
C23—C24—H24119.6C37A—C38A—H38A119.9
C25—C24—C23120.8 (3)C37A—C38A—C39A120.3 (3)
C25—C24—H24119.6C39A—C38A—H38A119.9
C20—C25—H25120.3C34A—C39A—C38A119.8 (3)
C24—C25—C20119.5 (3)C34A—C39A—H39A120.1
C24—C25—H25120.3C38A—C39A—H39A120.1
N15—C26—C27124.95 (19)N23A—C40A—N26A109.8 (2)
N18—C26—N15112.05 (18)N23A—C40A—C41A126.3 (2)
N18—C26—C27123.0 (2)N26A—C40A—C41A123.9 (2)
C28—C27—C26119.4 (2)C42A—C41A—C40A120.2 (2)
C32—C27—C26121.3 (2)C46A—C41A—C40A120.8 (2)
C32—C27—C28119.4 (2)C46A—C41A—C42A119.0 (2)
C27—C28—H28119.9C41A—C42A—H42A119.9
C29—C28—C27120.1 (2)C43A—C42A—C41A120.2 (3)
C29—C28—H28119.9C43A—C42A—H42A119.9
C28—C29—H29119.9C42A—C43A—H43A119.7
C28—C29—C30120.2 (2)C42A—C43A—C44A120.6 (3)
C30—C29—H29119.9C44A—C43A—H43A119.7
C29—C30—H30120.0C43A—C44A—H44A120.1
C29—C30—C31120.0 (2)C45A—C44A—C43A119.8 (3)
C31—C30—H30120.0C45A—C44A—H44A120.1
C30—C31—H31119.9C44A—C45A—H45A120.1
C32—C31—C30120.1 (2)C44A—C45A—C46A119.7 (3)
C32—C31—H31119.9C46A—C45A—H45A120.1
C27—C32—H32119.9C41A—C46A—H46A119.6
C31—C32—C27120.2 (2)C45A—C46A—C41A120.7 (2)
C31—C32—H32119.9C45A—C46A—H46A119.6
N19—C33—C34124.9 (2)N27A—C47A—H47D109.5
N22—C33—N19112.1 (2)N27A—C47A—H47E109.5
N22—C33—C34123.1 (2)N27A—C47A—H47F109.5
C35—C34—C33120.7 (2)H47D—C47A—H47E109.5
C35—C34—C39119.6 (2)H47D—C47A—H47F109.5
C39—C34—C33119.6 (2)H47E—C47A—H47F109.5
C34—C35—H35120.3N27A—C48A—H48D109.5
C34—C35—C36119.5 (3)N27A—C48A—H48E109.5
C36—C35—H35120.3N27A—C48A—H48F109.5
C35—C36—H36119.6H48D—C48A—H48E109.5
C37—C36—C35120.7 (3)H48D—C48A—H48F109.5
C37—C36—H36119.6H48E—C48A—H48F109.5
C36—C37—H37120.1N28A—C49A—H49D109.5
C38—C37—C36119.9 (3)N28A—C49A—H49E109.5
C38—C37—H37120.1N28A—C49A—H49F109.5
C37—C38—H38119.9H49D—C49A—H49E109.5
C37—C38—C39120.2 (3)H49D—C49A—H49F109.5
C39—C38—H38119.9H49E—C49A—H49F109.5
C34—C39—H39119.9N28A—C50A—H50D109.5
C38—C39—C34120.2 (2)N28A—C50A—H50E109.5
C38—C39—H39119.9N28A—C50A—H50F109.5
N23—C40—N26110.0 (2)H50D—C50A—H50E109.5
N23—C40—C41126.4 (2)H50D—C50A—H50F109.5
N26—C40—C41123.5 (2)H50E—C50A—H50F109.5
C42—C41—C40120.3 (2)Cl1—C25S—H25B109.5
C46—C41—C40120.8 (2)Cl1—C25S—H25C109.5
C46—C41—C42118.9 (2)Cl2—C25S—Cl1110.9 (6)
C41—C42—H42119.7Cl2—C25S—H25B109.5
C43—C42—C41120.6 (2)Cl2—C25S—H25C109.5
C43—C42—H42119.7H25B—C25S—H25C108.0
C42—C43—H43119.9Cl3—C26S—H26A108.7
C44—C43—C42120.2 (3)Cl3—C26S—H26B108.7
C44—C43—H43119.9Cl4—C26S—Cl3114.2 (5)
C43—C44—H44120.1Cl4—C26S—H26A108.7
C43—C44—C45119.9 (2)Cl4—C26S—H26B108.7
C45—C44—H44120.1H26A—C26S—H26B107.6
C44—C45—H45119.9C2S—C1S—H1S119.7
C46—C45—C44120.3 (2)C6S—C1S—H1S119.7
C46—C45—H45119.9C6S—C1S—C2S120.7 (3)
C41—C46—H46119.9C1S—C2S—H2S120.2
C45—C46—C41120.2 (2)C3S—C2S—C1S119.5 (3)
C45—C46—H46119.9C3S—C2S—H2S120.2
N27—C47—H47A109.5C2S—C3S—H3S119.9
N27—C47—H47B109.5C2S—C3S—C4S120.2 (3)
N27—C47—H47C109.5C4S—C3S—H3S119.9
H47A—C47—H47B109.5C3S—C4S—H4S120.1
H47A—C47—H47C109.5C5S—C4S—C3S119.8 (3)
H47B—C47—H47C109.5C5S—C4S—H4S120.1
N27—C48—H48A109.5C4S—C5S—H5S119.9
N27—C48—H48B109.5C6S—C5S—C4S120.2 (3)
N27—C48—H48C109.5C6S—C5S—H5S119.9
H48A—C48—H48B109.5C1S—C6S—C5S119.7 (3)
H48A—C48—H48C109.5C1S—C6S—H6S120.2
H48B—C48—H48C109.5C5S—C6S—H6S120.2
N28—C49—H49A109.5C8S—C7S—H7S120.0
N28—C49—H49B109.5C8S—C7S—C12S120.0
N28—C49—H49C109.5C12S—C7S—H7S120.0
H49A—C49—H49B109.5C7S—C8S—H8S120.0
H49A—C49—H49C109.5C7S—C8S—C9S120.0
H49B—C49—H49C109.5C9S—C8S—H8S120.0
N28—C50—H50A109.5C8S—C9S—H9S120.0
N28—C50—H50B109.5C10S—C9S—C8S120.0
N28—C50—H50C109.5C10S—C9S—H9S120.0
H50A—C50—H50B109.5C9S—C10S—H10S120.0
H50A—C50—H50C109.5C9S—C10S—C11S120.0
H50B—C50—H50C109.5C11S—C10S—H10S120.0
N2A—Zr1A—N6A135.77 (7)C10S—C11S—H11S120.0
N2A—Zr1A—N10A74.36 (7)C10S—C11S—C12S120.0
N2A—Zr1A—N12A137.39 (6)C12S—C11S—H11S120.0
N2A—Zr1A—N16A71.45 (6)C7S—C12S—H12S120.0
N2A—Zr1A—N20A80.57 (7)C11S—C12S—C7S120.0
N6A—Zr1A—N10A72.87 (7)C11S—C12S—H12S120.0
N6A—Zr1A—N12A72.47 (7)C14S—C13S—H13S120.0
N6A—Zr1A—N16A141.64 (7)C14S—C13S—C18S120.0
N6A—Zr1A—N20A76.90 (6)C18S—C13S—H13S120.0
N9A—Zr1A—N2A114.04 (8)C13S—C14S—H14S120.0
N9A—Zr1A—N6A94.15 (8)C15S—C14S—C13S120.0
N9A—Zr1A—N10A88.78 (7)C15S—C14S—H14S120.0
N9A—Zr1A—N12A88.63 (7)C14S—C15S—H15S120.0
N9A—Zr1A—N16A95.60 (8)C14S—C15S—C16S120.0
N9A—Zr1A—N20A164.65 (7)C16S—C15S—H15S120.0
N12A—Zr1A—N10A144.95 (6)C15S—C16S—H16S120.0
N16A—Zr1A—N10A144.23 (6)C17S—C16S—C15S120.0
N16A—Zr1A—N12A70.78 (6)C17S—C16S—H16S120.0
N16A—Zr1A—N20A84.41 (6)C16S—C17S—H17S120.0
N20A—Zr1A—N10A100.20 (7)C16S—C17S—C18S120.0
N20A—Zr1A—N12A76.85 (6)C18S—C17S—H17S120.0
N13A—Zr2A—N17A74.78 (7)C13S—C18S—H18S120.0
N13A—Zr2A—N21A76.58 (6)C17S—C18S—C13S120.0
N13A—Zr2A—N27A151.06 (7)C17S—C18S—H18S120.0
N21A—Zr2A—N17A80.90 (7)C20S—C19S—H19S120.0
N23A—Zr2A—N13A87.66 (7)C20S—C19S—C24S120.0
N23A—Zr2A—N17A83.96 (7)C24S—C19S—H19S120.0
N23A—Zr2A—N21A160.50 (7)C19S—C20S—H20S120.0
N23A—Zr2A—N27A117.29 (7)C19S—C20S—C21S120.0
N24A—Zr2A—N13A122.34 (7)C21S—C20S—H20S120.0
N24A—Zr2A—N17A90.66 (7)C20S—C21S—H21S120.0
N24A—Zr2A—N21A156.60 (7)C22S—C21S—C20S120.0
N24A—Zr2A—N23A34.83 (7)C22S—C21S—H21S120.0
N24A—Zr2A—N27A82.91 (7)C21S—C22S—H22S120.0
N27A—Zr2A—N17A92.54 (7)C23S—C22S—C21S120.0
N27A—Zr2A—N21A75.76 (7)C23S—C22S—H22S120.0
N28A—Zr2A—N13A86.95 (8)C22S—C23S—H23S120.0
N28A—Zr2A—N17A160.63 (8)C22S—C23S—C24S120.0
N28A—Zr2A—N21A88.76 (8)C24S—C23S—H23S120.0
N28A—Zr2A—N23A101.97 (8)C19S—C24S—H24S120.0
N28A—Zr2A—N24A104.79 (8)C23S—C24S—C19S120.0
N28A—Zr2A—N27A100.78 (8)C23S—C24S—H24S120.0
Zr1—N2—N3—N4172.54 (14)Zr2A—N24A—N25A—N26A123.9 (9)
Zr1—N6—N7—N8158.33 (15)N1A—N2A—N3A—N4A0.4 (3)
Zr1—N12—N13—Zr218.5 (3)N1A—C1A—C2A—C3A1.8 (4)
Zr1—N12—N13—N14174.03 (13)N1A—C1A—C2A—C7A177.6 (2)
Zr1—N16—N17—Zr226.3 (3)N2A—N1A—C1A—N4A0.0 (2)
Zr1—N16—N17—N18170.36 (14)N2A—N1A—C1A—C2A179.5 (2)
Zr1—N20—N21—Zr216.6 (3)N2A—N3A—N4A—C1A0.4 (2)
Zr1—N20—N21—N22177.97 (14)N3A—N4A—C1A—N1A0.3 (3)
Zr2—N13—N14—C19172.49 (14)N3A—N4A—C1A—C2A179.8 (2)
Zr2—N17—N18—C26166.46 (14)N4A—C1A—C2A—C3A177.6 (2)
Zr2—N21—N22—C33167.53 (13)N4A—C1A—C2A—C7A3.0 (4)
Zr2—N23—N24—N25173.82 (19)N5A—N6A—N7A—N8A0.3 (3)
N1—N2—N3—N40.5 (2)N5A—C8A—C9A—C10A156.5 (2)
N1—C1—C2—C310.5 (4)N5A—C8A—C9A—C14A21.9 (4)
N1—C1—C2—C7169.5 (2)N6A—N5A—C8A—N8A0.7 (3)
N2—N1—C1—N40.1 (2)N6A—N5A—C8A—C9A177.4 (2)
N2—N1—C1—C2179.4 (2)N6A—N7A—N8A—C8A0.1 (2)
N2—N3—N4—C10.5 (2)N7A—N8A—C8A—N5A0.5 (3)
N3—N4—C1—N10.4 (3)N7A—N8A—C8A—C9A177.6 (2)
N3—N4—C1—C2179.6 (2)N8A—C8A—C9A—C10A21.4 (4)
N4—C1—C2—C3168.7 (2)N8A—C8A—C9A—C14A160.3 (2)
N4—C1—C2—C711.3 (4)N11A—N12A—N13A—Zr2A158.69 (16)
N5—N6—N7—N80.3 (2)N11A—N12A—N13A—N14A0.2 (2)
N5—C8—C9—C10155.0 (3)N11A—C19A—C20A—C21A10.1 (4)
N5—C8—C9—C1422.7 (4)N11A—C19A—C20A—C25A171.0 (2)
N6—N5—C8—N81.3 (3)N12A—N11A—C19A—N14A0.4 (3)
N6—N5—C8—C9176.4 (2)N12A—N11A—C19A—C20A175.9 (2)
N6—N7—N8—C80.5 (3)N12A—N13A—N14A—C19A0.4 (2)
N7—N8—C8—N51.2 (3)N13A—N14A—C19A—N11A0.5 (3)
N7—N8—C8—C9176.5 (2)N13A—N14A—C19A—C20A175.9 (2)
N8—C8—C9—C1022.4 (4)N14A—C19A—C20A—C21A165.9 (2)
N8—C8—C9—C14159.8 (2)N14A—C19A—C20A—C25A13.0 (4)
N11—N12—N13—Zr2168.14 (18)N15A—N16A—N17A—Zr2A171.18 (16)
N11—N12—N13—N140.7 (2)N15A—N16A—N17A—N18A0.5 (2)
N11—C19—C20—C216.1 (4)N15A—C26A—C27A—C28A161.6 (2)
N11—C19—C20—C25175.3 (2)N15A—C26A—C27A—C32A16.8 (3)
N12—N11—C19—N140.7 (2)N16A—N15A—C26A—N18A0.4 (2)
N12—N11—C19—C20178.0 (2)N16A—N15A—C26A—C27A176.6 (2)
N12—N13—N14—C190.2 (2)N16A—N17A—N18A—C26A0.3 (2)
N13—N14—C19—N110.3 (2)N17A—N18A—C26A—N15A0.1 (2)
N13—N14—C19—C20178.5 (2)N17A—N18A—C26A—C27A176.8 (2)
N14—C19—C20—C21175.3 (3)N18A—C26A—C27A—C28A15.0 (4)
N14—C19—C20—C253.3 (4)N18A—C26A—C27A—C32A166.7 (2)
N15—N16—N17—Zr2163.00 (15)N19A—N20A—N21A—Zr2A170.00 (14)
N15—N16—N17—N180.4 (2)N19A—N20A—N21A—N22A0.1 (2)
N15—C26—C27—C28168.6 (2)N19A—C33A—C34A—C35A0.3 (4)
N15—C26—C27—C3212.3 (3)N19A—C33A—C34A—C39A179.9 (2)
N16—N15—C26—N180.4 (2)N20A—N19A—C33A—N22A0.4 (2)
N16—N15—C26—C27177.5 (2)N20A—N19A—C33A—C34A179.8 (2)
N16—N17—N18—C260.6 (2)N20A—N21A—N22A—C33A0.3 (2)
N17—N18—C26—N150.6 (2)N21A—N22A—C33A—N19A0.5 (2)
N17—N18—C26—C27177.3 (2)N21A—N22A—C33A—C34A179.9 (2)
N18—C26—C27—C2813.7 (3)N22A—C33A—C34A—C35A179.1 (2)
N18—C26—C27—C32165.4 (2)N22A—C33A—C34A—C39A0.5 (3)
N19—N20—N21—Zr2165.14 (14)N23A—N24A—N25A—N26A0.0 (3)
N19—N20—N21—N220.3 (2)N23A—C40A—C41A—C42A176.1 (2)
N19—C33—C34—C359.1 (4)N23A—C40A—C41A—C46A4.7 (4)
N19—C33—C34—C39172.0 (2)N24A—N23A—C40A—N26A0.5 (3)
N20—N19—C33—N220.1 (2)N24A—N23A—C40A—C41A179.5 (2)
N20—N19—C33—C34177.9 (2)N24A—N25A—N26A—C40A0.3 (3)
N20—N21—N22—C330.3 (2)N25A—N26A—C40A—N23A0.5 (3)
N21—N22—C33—N190.1 (2)N25A—N26A—C40A—C41A179.6 (2)
N21—N22—C33—C34177.77 (19)N26A—C40A—C41A—C42A4.9 (4)
N22—C33—C34—C35168.5 (2)N26A—C40A—C41A—C46A174.3 (2)
N22—C33—C34—C3910.4 (3)C1A—N1A—N2A—Zr1A178.62 (14)
N23—N24—N25—N260.2 (3)C1A—N1A—N2A—N3A0.2 (2)
N23—C40—C41—C42176.3 (2)C1A—C2A—C3A—C4A179.7 (2)
N23—C40—C41—C465.3 (4)C1A—C2A—C7A—C6A179.4 (2)
N24—N23—C40—N260.1 (3)C21A—C20A—C25A—C24A1.6 (4)
N24—N23—C40—C41177.8 (2)C21A—C22A—C23A—C24A1.0 (4)
N24—N25—N26—C400.1 (3)C2A—C3A—C4A—C5A0.7 (4)
N25—N26—C40—N230.0 (3)C3A—C2A—C7A—C6A0.0 (4)
N25—N26—C40—C41178.0 (2)C3A—C4A—C5A—C6A0.8 (4)
N26—C40—C41—C426.0 (4)C4A—C5A—C6A—C7A0.5 (4)
N26—C40—C41—C46172.4 (2)C5A—C6A—C7A—C2A0.1 (4)
C1—N1—N2—Zr1172.68 (14)C7A—C2A—C3A—C4A0.3 (4)
C1—N1—N2—N30.3 (2)C8A—N5A—N6A—Zr1A169.77 (14)
C1—C2—C3—C4179.7 (2)C8A—N5A—N6A—N7A0.6 (2)
C1—C2—C7—C6180.0 (2)C8A—C9A—C10A—C11A176.9 (2)
C2—C3—C4—C50.4 (4)C8A—C9A—C14A—C13A177.7 (2)
C3—C2—C7—C60.0 (4)C9A—C10A—C11A—C12A0.7 (4)
C3—C4—C5—C60.3 (4)C10A—C9A—C14A—C13A0.6 (4)
C4—C5—C6—C70.0 (4)C10A—C11A—C12A—C13A1.0 (4)
C5—C6—C7—C20.1 (4)C11A—C12A—C13A—C14A1.8 (4)
C7—C2—C3—C40.2 (4)C12A—C13A—C14A—C9A1.0 (4)
C8—N5—N6—Zr1157.72 (15)C14A—C9A—C10A—C11A1.5 (4)
C8—N5—N6—N71.0 (2)C19A—N11A—N12A—Zr1A173.70 (14)
C8—C9—C10—C11177.8 (3)C19A—N11A—N12A—N13A0.1 (2)
C8—C9—C14—C13178.7 (2)C19A—C20A—C25A—C24A179.5 (2)
C9—C10—C11—C120.7 (5)C20A—C21A—C22A—C23A0.8 (4)
C10—C9—C14—C131.0 (4)C22A—C21A—C20A—C19A179.0 (2)
C10—C11—C12—C130.5 (5)C22A—C21A—C20A—C25A2.1 (4)
C11—C12—C13—C140.4 (4)C22A—C23A—C24A—C25A1.5 (4)
C12—C13—C14—C91.2 (4)C23A—C24A—C25A—C20A0.2 (4)
C14—C9—C10—C110.0 (4)C26A—N15A—N16A—Zr1A178.14 (14)
C19—N11—N12—Zr1173.71 (14)C26A—N15A—N16A—N17A0.5 (2)
C19—N11—N12—N130.8 (2)C26A—C27A—C28A—C29A178.1 (3)
C19—C20—C21—C22179.0 (3)C26A—C27A—C32A—C31A177.5 (2)
C19—C20—C25—C24179.3 (3)C27A—C28A—C29A—C30A0.9 (5)
C20—C21—C22—C230.2 (5)C28A—C27A—C32A—C31A0.9 (4)
C21—C20—C25—C240.7 (4)C28A—C29A—C30A—C31A1.5 (5)
C21—C22—C23—C240.4 (6)C29A—C30A—C31A—C32A0.9 (5)
C22—C23—C24—C250.0 (5)C30A—C31A—C32A—C27A0.3 (4)
C23—C24—C25—C200.5 (5)C32A—C27A—C28A—C29A0.2 (4)
C25—C20—C21—C220.3 (5)C33A—N19A—N20A—Zr1A171.93 (13)
C26—N15—N16—Zr1171.73 (13)C33A—N19A—N20A—N21A0.2 (2)
C26—N15—N16—N170.0 (2)C33A—C34A—C35A—C36A179.6 (3)
C26—C27—C28—C29179.2 (2)C33A—C34A—C39A—C38A179.3 (3)
C26—C27—C32—C31178.8 (2)C34A—C35A—C36A—C37A0.1 (5)
C27—C28—C29—C300.1 (4)C35A—C34A—C39A—C38A1.1 (4)
C28—C27—C32—C310.3 (3)C35A—C36A—C37A—C38A0.6 (5)
C28—C29—C30—C310.5 (4)C36A—C37A—C38A—C39A0.2 (5)
C29—C30—C31—C320.9 (4)C37A—C38A—C39A—C34A0.6 (5)
C30—C31—C32—C270.8 (4)C39A—C34A—C35A—C36A0.8 (4)
C32—C27—C28—C290.0 (3)C40A—N23A—N24A—Zr2A170.16 (17)
C33—N19—N20—Zr1178.37 (13)C40A—N23A—N24A—N25A0.3 (3)
C33—N19—N20—N210.2 (2)C40A—C41A—C42A—C43A178.6 (2)
C33—C34—C35—C36178.9 (3)C40A—C41A—C46A—C45A179.2 (2)
C33—C34—C39—C38178.3 (2)C41A—C42A—C43A—C44A0.8 (4)
C34—C35—C36—C370.9 (5)C42A—C41A—C46A—C45A0.0 (4)
C35—C34—C39—C380.6 (4)C42A—C43A—C44A—C45A0.5 (4)
C35—C36—C37—C381.1 (6)C43A—C44A—C45A—C46A0.1 (4)
C36—C37—C38—C390.5 (5)C44A—C45A—C46A—C41A0.3 (4)
C37—C38—C39—C340.4 (4)C46A—C41A—C42A—C43A0.5 (4)
C39—C34—C35—C360.0 (4)C1S—C2S—C3S—C4S0.4 (4)
C40—N23—N24—Zr2173.99 (16)C2S—C1S—C6S—C5S0.0 (4)
C40—N23—N24—N250.2 (2)C2S—C3S—C4S—C5S0.6 (4)
C40—C41—C42—C43178.2 (2)C3S—C4S—C5S—C6S1.3 (4)
C40—C41—C46—C45178.9 (2)C4S—C5S—C6S—C1S1.0 (4)
C41—C42—C43—C440.7 (4)C6S—C1S—C2S—C3S0.7 (4)
C42—C41—C46—C450.5 (4)C7S—C8S—C9S—C10S0.0
C42—C43—C44—C450.5 (4)C8S—C7S—C12S—C11S0.0
C43—C44—C45—C460.3 (4)C8S—C9S—C10S—C11S0.0
C44—C45—C46—C410.8 (4)C9S—C10S—C11S—C12S0.0
C46—C41—C42—C430.2 (4)C10S—C11S—C12S—C7S0.0
Zr1A—N2A—N3A—N4A178.42 (14)C12S—C7S—C8S—C9S0.0
Zr1A—N6A—N7A—N8A169.47 (14)C13S—C14S—C15S—C16S0.0
Zr1A—N12A—N13A—Zr2A28.4 (3)C14S—C13S—C18S—C17S0.0
Zr1A—N12A—N13A—N14A172.70 (14)C14S—C15S—C16S—C17S0.0
Zr1A—N16A—N17A—Zr2A7.3 (3)C15S—C16S—C17S—C18S0.0
Zr1A—N16A—N17A—N18A178.01 (14)C16S—C17S—C18S—C13S0.0
Zr1A—N20A—N21A—Zr2A19.6 (3)C18S—C13S—C14S—C15S0.0
Zr1A—N20A—N21A—N22A170.46 (14)C19S—C20S—C21S—C22S0.0
Zr2A—N13A—N14A—C19A163.67 (14)C20S—C19S—C24S—C23S0.0
Zr2A—N17A—N18A—C26A173.46 (14)C20S—C21S—C22S—C23S0.0
Zr2A—N21A—N22A—C33A171.94 (13)C21S—C22S—C23S—C24S0.0
Zr2A—N23A—N24A—N25A170.44 (19)C22S—C23S—C24S—C19S0.0
Zr2A—N23A—C40A—N26A56.7 (9)C24S—C19S—C20S—C21S0.0
Zr2A—N23A—C40A—C41A124.2 (8)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N10—H10···N50.85 (2)1.96 (2)2.732 (3)151 (2)
N27—H27···N220.84 (2)2.35 (2)2.965 (3)130 (2)
N10A—H10B···N5A0.85 (2)2.16 (2)2.902 (3)145 (2)
N27A—H27A···N22A0.85 (2)2.33 (2)2.940 (3)129 (2)
µ-Oxido-bis(µ-5-phenyltetrazolato-κ2N2:N3)\ bis[(dimethylamido)tris(5-phenyltetrazolato-κN2)tantalum(V)] toluene 0.25-solvate (3) top
Crystal data top
(C2H8N)2[Ta2(C7H5N4)8(C2H6N)2O]·0.25C7H8F(000) = 6964
Mr = 1742.47Dx = 1.539 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 22.5131 (8) ÅCell parameters from 91158 reflections
b = 25.5101 (9) Åθ = 2.3–29.1°
c = 26.7165 (9) ŵ = 2.98 mm1
β = 101.3830 (4)°T = 105 K
V = 15041.8 (9) Å3Block, yellow
Z = 80.39 × 0.32 × 0.24 mm
Data collection top
Bruker SMART APEX CCD area detector
diffractometer
29545 independent reflections
Radiation source: sealed tube25534 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
Detector resolution: 8 pixels mm-1θmax = 26.0°, θmin = 1.8°
ω and φ scansh = 2727
Absorption correction: multi-scan
(SADABS; Bruker, 2018)
k = 3130
Tmin = 0.4, Tmax = 0.5l = 3232
173076 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.068 w = 1/[σ2(Fo2) + (0.0298P)2 + 35.7711P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.007
29545 reflectionsΔρmax = 2.48 e Å3
1915 parametersΔρmin = 1.24 e Å3
79 restraints
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ta10.78099 (2)0.94792 (2)0.79238 (2)0.01469 (3)
Ta20.74252 (2)0.91178 (2)0.65793 (2)0.01519 (3)
O10.76194 (9)0.90565 (8)0.73102 (8)0.0153 (4)
N10.67073 (12)0.98108 (11)0.84250 (11)0.0193 (6)
N20.69683 (12)0.94095 (11)0.82225 (10)0.0185 (6)
N30.65957 (13)0.89992 (12)0.81262 (13)0.0275 (7)
N40.60817 (13)0.91288 (12)0.82675 (13)0.0292 (7)
N50.80972 (12)0.87098 (12)0.88725 (11)0.0213 (6)
N60.78700 (12)0.87496 (11)0.83714 (10)0.0180 (6)
N70.76471 (13)0.82945 (12)0.81798 (11)0.0242 (6)
N80.77283 (14)0.79436 (12)0.85588 (11)0.0256 (7)
N90.92147 (12)0.96424 (11)0.83791 (11)0.0197 (6)
N100.87845 (12)0.92979 (11)0.81737 (10)0.0185 (6)
N110.90236 (13)0.88290 (12)0.81292 (12)0.0251 (6)
N120.96129 (13)0.88549 (12)0.83045 (12)0.0260 (7)
N130.79424 (12)1.01515 (11)0.82530 (10)0.0184 (6)
N140.86383 (12)1.02821 (11)0.74126 (11)0.0182 (6)
N150.82675 (12)0.98755 (11)0.73422 (10)0.0167 (6)
N160.81155 (12)0.97630 (11)0.68477 (10)0.0176 (6)
N170.83841 (12)1.00968 (11)0.65811 (11)0.0193 (6)
N180.67607 (12)1.03450 (11)0.74570 (11)0.0203 (6)
N190.70844 (12)0.99327 (11)0.73745 (11)0.0186 (6)
N200.69345 (12)0.97906 (11)0.68876 (11)0.0188 (6)
N210.65025 (12)1.01033 (11)0.66414 (11)0.0211 (6)
N220.60300 (12)0.90994 (11)0.60742 (10)0.0190 (6)
N230.64588 (12)0.89017 (11)0.64458 (11)0.0191 (6)
N240.62186 (12)0.86451 (12)0.67870 (12)0.0247 (6)
N250.56221 (12)0.86681 (12)0.66476 (11)0.0243 (6)
N260.72941 (13)0.79831 (12)0.60770 (11)0.0236 (6)
N270.73978 (12)0.82504 (11)0.65197 (10)0.0196 (6)
N280.76376 (15)0.79373 (12)0.69040 (12)0.0301 (7)
N290.76860 (16)0.74581 (12)0.67199 (12)0.0304 (7)
N300.84918 (12)0.90238 (12)0.59743 (11)0.0211 (6)
N310.82797 (12)0.88601 (11)0.63810 (11)0.0187 (6)
N320.86789 (13)0.85609 (12)0.66852 (12)0.0246 (6)
N330.91654 (13)0.85224 (12)0.64756 (12)0.0266 (7)
N340.72447 (12)0.95314 (12)0.59642 (11)0.0205 (6)
N350.64569 (13)0.79255 (12)0.76311 (12)0.0268 (7)
H35B0.6442890.8104400.7334360.032*
H35C0.6733680.8086150.7877680.032*
N360.88190 (14)0.78445 (12)0.76317 (13)0.0311 (7)
H36B0.8804190.8123980.7840640.037*
H36C0.8561170.7910430.7330610.037*
C10.61626 (14)0.96213 (13)0.84464 (12)0.0195 (7)
C20.56820 (14)0.99352 (14)0.86073 (12)0.0204 (7)
C30.57101 (15)1.04780 (14)0.85999 (13)0.0224 (7)
H30.6054871.0645800.8517070.027*
C40.52421 (16)1.07772 (15)0.87116 (14)0.0268 (8)
H40.5264941.1148950.8705400.032*
C50.47382 (16)1.05329 (16)0.88331 (14)0.0297 (8)
H50.4412341.0737360.8904920.036*
C60.47103 (16)0.99914 (16)0.88496 (14)0.0281 (8)
H60.4367680.9826110.8939020.034*
C70.51796 (15)0.96864 (15)0.87366 (13)0.0229 (7)
H70.5158770.9314680.8747070.028*
C80.80033 (14)0.82073 (14)0.89758 (13)0.0205 (7)
C90.81943 (15)0.79595 (14)0.94777 (13)0.0220 (7)
C100.84377 (16)0.82556 (15)0.99044 (14)0.0269 (8)
H100.8472720.8624960.9875260.032*
C110.86302 (17)0.80141 (16)1.03735 (14)0.0297 (8)
H110.8796220.8219121.0664350.036*
C120.85821 (17)0.74792 (16)1.04203 (14)0.0294 (8)
H120.8716470.7314611.0741630.035*
C130.83370 (18)0.71835 (16)0.99966 (15)0.0321 (9)
H130.8301400.6814451.0028150.039*
C140.81423 (17)0.74206 (15)0.95251 (15)0.0293 (8)
H140.7973760.7214520.9235690.035*
C150.97205 (15)0.93540 (14)0.84566 (13)0.0206 (7)
C161.03290 (15)0.95550 (15)0.86742 (13)0.0232 (7)
C171.08101 (16)0.92040 (16)0.88275 (14)0.0270 (8)
H171.0744050.8836650.8796320.032*
C181.13812 (17)0.93985 (18)0.90245 (16)0.0370 (10)
H181.1708660.9161800.9125830.044*
C191.14842 (18)0.99319 (19)0.90767 (17)0.0405 (10)
H191.1878141.0060310.9216380.049*
C201.10103 (18)1.02764 (18)0.89243 (18)0.0412 (10)
H201.1078221.0643230.8959950.049*
C211.04357 (17)1.00893 (16)0.87193 (16)0.0323 (9)
H211.0113371.0328860.8609200.039*
C220.79369 (17)1.07116 (14)0.81602 (14)0.0264 (8)
H22A0.7830331.0777660.7792000.040*
H22B0.8339251.0856950.8296560.040*
H22C0.7637521.0878720.8329260.040*
C230.80943 (15)1.00180 (14)0.88000 (13)0.0232 (7)
H23A0.8494311.0160290.8949450.035*
H23B0.8099540.9636090.8839980.035*
H23C0.7789921.0168960.8974250.035*
C240.87044 (14)1.04135 (13)0.69410 (13)0.0184 (7)
C250.90677 (14)1.08673 (13)0.68413 (13)0.0184 (7)
C260.93104 (15)1.12008 (13)0.72404 (13)0.0207 (7)
H260.9238331.1135080.7573280.025*
C270.96558 (15)1.16271 (14)0.71565 (14)0.0235 (7)
H270.9821441.1853270.7431110.028*
C280.97604 (16)1.17244 (15)0.66709 (15)0.0284 (8)
H280.9993471.2020530.6612580.034*
C290.95277 (18)1.13933 (16)0.62717 (15)0.0333 (9)
H290.9603391.1459940.5940100.040*
C300.91817 (17)1.09614 (15)0.63557 (14)0.0282 (8)
H300.9023821.0731350.6082050.034*
C310.64054 (14)1.04421 (14)0.70026 (13)0.0217 (7)
C320.59486 (15)1.08617 (14)0.69033 (14)0.0237 (7)
C330.57201 (16)1.10708 (14)0.73043 (16)0.0291 (8)
H330.5881941.0964730.7644810.035*
C340.52532 (17)1.14364 (15)0.72083 (18)0.0351 (10)
H340.5091631.1575650.7483020.042*
C350.50252 (17)1.15966 (16)0.67173 (19)0.0402 (11)
H350.4702691.1842920.6653190.048*
C360.5263 (2)1.14006 (17)0.63149 (18)0.0433 (11)
H360.5113661.1521420.5977150.052*
C370.57202 (18)1.10279 (16)0.64060 (16)0.0355 (9)
H370.5877161.0886250.6129900.043*
C380.55178 (14)0.89463 (13)0.62075 (12)0.0178 (7)
C390.49076 (14)0.90553 (13)0.59108 (13)0.0186 (7)
C400.44038 (15)0.88391 (14)0.60693 (13)0.0224 (7)
H400.4457090.8617000.6360170.027*
C410.38281 (16)0.89509 (15)0.57996 (15)0.0274 (8)
H410.3485350.8811530.5911610.033*
C420.37463 (16)0.92630 (16)0.53694 (15)0.0318 (9)
H420.3348810.9338110.5187150.038*
C430.42458 (17)0.94672 (16)0.52033 (15)0.0313 (9)
H430.4191410.9674580.4902310.038*
C440.48232 (16)0.93674 (15)0.54779 (14)0.0249 (8)
H440.5164220.9514000.5368850.030*
C450.74726 (14)0.74971 (13)0.62146 (13)0.0192 (7)
C460.74600 (15)0.70509 (13)0.58607 (13)0.0208 (7)
C470.7125 (2)0.70717 (16)0.53689 (15)0.0351 (9)
H470.6901990.7379560.5253750.042*
C480.7111 (2)0.66473 (17)0.50403 (16)0.0455 (12)
H480.6870920.6662040.4705460.055*
C490.7445 (2)0.62057 (16)0.52016 (15)0.0354 (9)
H490.7437750.5915580.4977480.042*
C500.77918 (17)0.61839 (15)0.56893 (16)0.0315 (9)
H500.8025370.5879820.5798120.038*
C510.78007 (16)0.66019 (15)0.60199 (15)0.0276 (8)
H510.8038440.6583870.6355320.033*
C520.90386 (15)0.88046 (13)0.60430 (13)0.0204 (7)
C530.9427 (3)0.8923 (3)0.5670 (3)0.019 (2)0.52 (2)
C540.9259 (3)0.9295 (4)0.5288 (3)0.021 (2)0.52 (2)
H540.8875470.9463010.5248910.025*0.52 (2)
C550.9651 (4)0.9423 (4)0.49653 (19)0.027 (2)0.52 (2)
H550.9535810.9677880.4704930.032*0.52 (2)
C561.0212 (4)0.9178 (4)0.5023 (3)0.029 (2)0.52 (2)
H561.0479960.9265230.4802400.034*0.52 (2)
C571.0380 (4)0.8805 (3)0.5404 (4)0.029 (2)0.52 (2)
H571.0763780.8637690.5443840.034*0.52 (2)
C580.9988 (4)0.8678 (3)0.5727 (4)0.030 (2)0.52 (2)
H581.0103440.8422800.5987810.036*0.52 (2)
C53B0.9510 (3)0.8850 (4)0.5731 (3)0.020 (3)0.48 (2)
C54B0.9369 (3)0.9145 (4)0.5286 (3)0.022 (2)0.48 (2)
H54B0.8976050.9291550.5184580.027*0.48 (2)
C55B0.9804 (4)0.9227 (5)0.4990 (2)0.027 (3)0.48 (2)
H55B0.9708090.9429030.4686500.032*0.48 (2)
C56B1.0380 (4)0.9013 (5)0.5139 (3)0.029 (3)0.48 (2)
H56B1.0677200.9068950.4937110.035*0.48 (2)
C57B1.0521 (3)0.8718 (3)0.5584 (4)0.032 (3)0.48 (2)
H57B1.0914280.8571390.5685800.038*0.48 (2)
C58B1.0086 (3)0.8636 (3)0.5880 (4)0.022 (2)0.48 (2)
H58B1.0182240.8433900.6183890.027*0.48 (2)
C590.71463 (17)1.00705 (15)0.57857 (14)0.0274 (8)
H59A0.7340671.0125500.5492490.041*
H59B0.7321591.0311470.6061180.041*
H59C0.6710391.0136980.5683630.041*
C600.71215 (16)0.91489 (15)0.55483 (13)0.0248 (8)
H60A0.6704270.9191820.5360360.037*
H60B0.7175060.8793710.5689760.037*
H60C0.7402810.9205070.5316380.037*
C610.58513 (17)0.79503 (16)0.77741 (16)0.0328 (9)
H61A0.5547120.7794330.7501580.049*
H61B0.5745520.8316960.7822510.049*
H61C0.5862310.7756040.8092210.049*
C620.66572 (18)0.73832 (16)0.75659 (18)0.0370 (10)
H62A0.6685480.7191230.7887510.056*
H62B0.7055180.7388960.7469530.056*
H62C0.6363910.7209260.7297420.056*
C630.8606 (2)0.73747 (17)0.7866 (2)0.0443 (11)
H63A0.8597540.7075330.7634990.066*
H63B0.8198120.7437840.7929290.066*
H63C0.8882400.7298790.8190220.066*
C640.94420 (19)0.77971 (17)0.75350 (17)0.0371 (9)
H64A0.9728170.7756940.7860450.056*
H64B0.9543430.8113000.7360760.056*
H64C0.9466740.7489890.7319840.056*
Ta1A0.26714 (2)0.72176 (2)0.71402 (2)0.01344 (3)
Ta2A0.29513 (2)0.74260 (2)0.85171 (2)0.01326 (3)
O1A0.27922 (9)0.75693 (8)0.77928 (8)0.0142 (4)
N1A0.13400 (12)0.70670 (11)0.65006 (10)0.0184 (6)
N2A0.16996 (12)0.73609 (11)0.68461 (11)0.0199 (6)
N3A0.14053 (13)0.77740 (12)0.69751 (12)0.0275 (7)
N4A0.08356 (13)0.77494 (13)0.67209 (13)0.0303 (7)
N5A0.23949 (12)0.81042 (11)0.62773 (10)0.0194 (6)
N6A0.25839 (12)0.79982 (11)0.67745 (10)0.0192 (6)
N7A0.26897 (14)0.84346 (12)0.70444 (12)0.0278 (7)
N8A0.25557 (15)0.88409 (12)0.67244 (12)0.0288 (7)
N9A0.38677 (12)0.70156 (11)0.66938 (10)0.0175 (6)
N10A0.35469 (12)0.73677 (11)0.69102 (10)0.0168 (6)
N11A0.38599 (13)0.78081 (11)0.70247 (12)0.0241 (6)
N12A0.43915 (13)0.77517 (12)0.68886 (12)0.0248 (6)
N13A0.25854 (12)0.65860 (10)0.67350 (10)0.0162 (5)
N18A0.17617 (12)0.63601 (11)0.75149 (10)0.0180 (6)
N19A0.21718 (11)0.67334 (11)0.76438 (10)0.0164 (5)
N20A0.22933 (12)0.67997 (10)0.81466 (10)0.0167 (6)
N21A0.19661 (12)0.64639 (11)0.83615 (11)0.0192 (6)
N14A0.36445 (12)0.63040 (10)0.75573 (10)0.0170 (6)
N15A0.33665 (11)0.67364 (10)0.76658 (10)0.0153 (5)
N16A0.34704 (12)0.68041 (10)0.81706 (10)0.0166 (5)
N17A0.38166 (12)0.64206 (11)0.84009 (10)0.0182 (6)
N22A0.18552 (12)0.73668 (11)0.90947 (10)0.0186 (6)
N23A0.20570 (12)0.75949 (11)0.87101 (10)0.0177 (6)
N24A0.16173 (13)0.78632 (13)0.84101 (13)0.0298 (7)
N25A0.11198 (13)0.78163 (13)0.86037 (13)0.0307 (7)
N26A0.32430 (12)0.85444 (11)0.90694 (10)0.0196 (6)
N27A0.29329 (12)0.82800 (11)0.86626 (10)0.0180 (6)
N28A0.26022 (13)0.86109 (12)0.83374 (11)0.0251 (6)
N29A0.26961 (13)0.90938 (11)0.85203 (12)0.0248 (6)
N30A0.43523 (12)0.75290 (11)0.90586 (10)0.0174 (6)
N31A0.39034 (11)0.76951 (10)0.86839 (10)0.0155 (5)
N32A0.40948 (12)0.80781 (12)0.84174 (11)0.0226 (6)
N33A0.46722 (12)0.81703 (12)0.86116 (11)0.0236 (6)
N34A0.30935 (12)0.69495 (11)0.90885 (10)0.0171 (6)
N35A0.14406 (13)0.86915 (11)0.76003 (11)0.0231 (6)
H35D0.1548470.8464800.7370790.028*
H35E0.1657630.8606890.7914520.028*
N36A0.38820 (13)0.88081 (12)0.76051 (12)0.0259 (7)
H36D0.3659670.8634380.7334120.031*
H36E0.3880130.8612400.7889630.031*
C1A0.08082 (15)0.73124 (13)0.64343 (13)0.0202 (7)
C2A0.02598 (15)0.71488 (13)0.60712 (13)0.0206 (7)
C3A0.02972 (16)0.68132 (14)0.56685 (13)0.0237 (7)
H3A0.0678780.6675740.5632860.028*
C4A0.02221 (17)0.66786 (15)0.53183 (14)0.0281 (8)
H4A0.0196190.6450680.5042240.034*
C5A0.07799 (17)0.68786 (15)0.53732 (15)0.0308 (9)
H5A0.1135880.6784520.5135460.037*
C6A0.08192 (16)0.72116 (15)0.57696 (16)0.0326 (9)
H6A0.1202010.7348100.5802920.039*
C7A0.03028 (16)0.73500 (15)0.61219 (15)0.0270 (8)
H7A0.0331900.7580060.6395610.032*
C8A0.23703 (15)0.86233 (14)0.62615 (13)0.0210 (7)
C9A0.21752 (15)0.89393 (14)0.57955 (14)0.0238 (7)
C10A0.21072 (14)0.87161 (14)0.53135 (13)0.0229 (7)
H10A0.2193010.8354620.5280070.028*
C11A0.19141 (16)0.90192 (16)0.48800 (14)0.0298 (8)
H11A0.1872300.8865090.4551240.036*
C12A0.17826 (18)0.95440 (17)0.49252 (15)0.0342 (9)
H12A0.1641280.9748830.4628650.041*
C13A0.1858 (2)0.97693 (17)0.54033 (16)0.0405 (10)
H13A0.1774711.0131740.5434280.049*
C14A0.2053 (2)0.94704 (16)0.58403 (16)0.0357 (9)
H14A0.2103960.9628110.6168100.043*
C15A0.43839 (14)0.72680 (13)0.66868 (12)0.0183 (7)
C16A0.48935 (15)0.70549 (14)0.64756 (12)0.0205 (7)
C17A0.53079 (16)0.74017 (15)0.63326 (15)0.0279 (8)
H17A0.5261190.7768430.6373100.033*
C18A0.57896 (17)0.72121 (16)0.61308 (16)0.0319 (9)
H18A0.6071600.7449690.6033790.038*
C19A0.58592 (17)0.66808 (16)0.60711 (15)0.0316 (9)
H19A0.6187370.6552310.5931080.038*
C20A0.54523 (19)0.63356 (17)0.62148 (17)0.0375 (10)
H20A0.5501570.5969200.6174040.045*
C21A0.49685 (17)0.65217 (15)0.64197 (15)0.0295 (8)
H21A0.4691090.6282260.6520700.035*
C22A0.25478 (16)0.60210 (13)0.67613 (13)0.0228 (7)
H22D0.2634030.5909880.7119480.034*
H22E0.2844480.5863280.6582990.034*
H22F0.2139400.5906860.6599220.034*
C23A0.25146 (15)0.67814 (14)0.62072 (12)0.0209 (7)
H23D0.2849940.6652520.6056340.031*
H23E0.2517230.7165510.6209190.031*
H23F0.2129620.6655870.6005160.031*
C31A0.16464 (14)0.61984 (13)0.79628 (13)0.0186 (7)
C32A0.12045 (15)0.57897 (13)0.80175 (13)0.0202 (7)
C33A0.08205 (15)0.55939 (13)0.75887 (14)0.0225 (7)
H33A0.0861030.5706490.7258160.027*
C34A0.03751 (16)0.52318 (14)0.76432 (15)0.0260 (8)
H34A0.0110330.5097690.7349750.031*
C35A0.03181 (16)0.50673 (14)0.81247 (16)0.0283 (8)
H35A0.0009160.4824830.8161030.034*
C36A0.07049 (19)0.52521 (16)0.85504 (16)0.0355 (9)
H36A0.0670490.5129930.8879370.043*
C37A0.11467 (18)0.56177 (16)0.85006 (15)0.0330 (9)
H37A0.1409340.5750530.8795850.040*
C24A0.39164 (14)0.61164 (13)0.80118 (12)0.0177 (7)
C25A0.42659 (15)0.56266 (13)0.80780 (13)0.0197 (7)
C30A0.4372 (2)0.53736 (15)0.85475 (15)0.0341 (9)
H30A0.4215120.5516420.8823390.041*
C29A0.4705 (2)0.49138 (16)0.86147 (15)0.0398 (10)
H29A0.4772360.4739010.8934910.048*
C28A0.49391 (17)0.47089 (14)0.82141 (15)0.0296 (8)
H28A0.5178310.4399450.8262380.036*
C27A0.48240 (15)0.49559 (14)0.77435 (14)0.0242 (7)
H27A0.4979010.4810940.7467750.029*
C26A0.44857 (14)0.54115 (13)0.76712 (13)0.0205 (7)
H26A0.4403680.5576900.7346270.025*
C38A0.12797 (15)0.75121 (13)0.90228 (13)0.0192 (7)
C39A0.08618 (15)0.73592 (14)0.93581 (13)0.0222 (7)
C40A0.03213 (17)0.76313 (16)0.93421 (16)0.0303 (8)
H40A0.0217980.7916310.9112490.036*
C41A0.00674 (18)0.74835 (18)0.96645 (18)0.0393 (10)
H41A0.0436150.7668010.9654200.047*
C42A0.00833 (19)0.70690 (19)0.99990 (16)0.0393 (10)
H42A0.0182440.6969431.0217930.047*
C43A0.06179 (18)0.67998 (18)1.00159 (15)0.0355 (9)
H43A0.0718600.6514341.0245410.043*
C44A0.10100 (16)0.69446 (15)0.96983 (14)0.0267 (8)
H44A0.1379810.6760280.9713400.032*
C45A0.30932 (14)0.90431 (13)0.89672 (12)0.0169 (6)
C46A0.33240 (14)0.94901 (13)0.92958 (13)0.0190 (7)
C51A0.31297 (16)0.99956 (14)0.91548 (14)0.0256 (8)
H51A0.2841601.0051990.8848220.031*
C50A0.33554 (19)1.04177 (15)0.94603 (16)0.0333 (9)
H50A0.3216671.0761460.9362670.040*
C49A0.37789 (19)1.03455 (15)0.99045 (15)0.0333 (9)
H49A0.3933911.0636651.0111230.040*
C48A0.39740 (19)0.98431 (16)1.00437 (15)0.0334 (9)
H48A0.4265400.9788751.0348720.040*
C47A0.37489 (17)0.94183 (14)0.97430 (14)0.0257 (8)
H47A0.3886410.9074880.9843590.031*
C52A0.48212 (15)0.78308 (13)0.90026 (12)0.0181 (7)
C53A0.54360 (14)0.78027 (13)0.93194 (13)0.0199 (7)
C58A0.58885 (16)0.81337 (15)0.92083 (14)0.0268 (8)
H58A0.5796710.8374970.8932970.032*
C57A0.64684 (17)0.81102 (17)0.94981 (16)0.0343 (9)
H57A0.6773560.8335700.9420300.041*
C56A0.66094 (16)0.77606 (17)0.99014 (15)0.0329 (9)
H56A0.7009870.7744181.0097520.040*
C55A0.61601 (17)0.74341 (16)1.00168 (15)0.0300 (8)
H55A0.6252720.7197571.0295970.036*
C54A0.55746 (16)0.74526 (14)0.97245 (14)0.0245 (8)
H54A0.5270280.7225950.9802100.029*
C59A0.31041 (17)0.64000 (14)0.92362 (14)0.0250 (8)
H59D0.3505140.6311640.9435880.037*
H59E0.3017880.6180650.8929240.037*
H59F0.2796570.6337690.9442800.037*
C60A0.32171 (15)0.73029 (13)0.95311 (12)0.0200 (7)
H60D0.2917690.7243230.9746100.030*
H60E0.3191860.7667420.9412940.030*
H60F0.3624300.7233890.9729480.030*
C61A0.07900 (16)0.86250 (15)0.76007 (14)0.0276 (8)
H61D0.0661190.8890480.7822090.041*
H61E0.0719870.8274730.7728040.041*
H61F0.0556740.8665630.7252210.041*
C62A0.16001 (17)0.92300 (16)0.74715 (18)0.0378 (10)
H62D0.1355900.9329710.7139700.057*
H62E0.2030860.9244370.7455120.057*
H62F0.1519360.9472980.7734210.057*
C63A0.35920 (18)0.93188 (17)0.76607 (17)0.0361 (9)
H63D0.3838360.9515060.7942530.054*
H63E0.3186930.9260700.7733090.054*
H63F0.3558280.9519200.7343440.054*
C64A0.45147 (16)0.88582 (15)0.75288 (15)0.0277 (8)
H64D0.4521400.9072920.7225880.042*
H64E0.4677450.8509380.7481280.042*
H64F0.4763110.9025230.7828980.042*
C1S1.0077 (4)1.1023 (2)1.0167 (4)0.065 (3)*0.5
H1SA0.9676721.1188361.0089210.098*0.5
H1SB1.0259231.1079621.0527360.098*0.5
H1SC1.0337301.1177850.9952260.098*0.5
C2S1.0013 (3)1.0443 (2)1.0062 (3)0.073 (3)*0.5
C3S0.9442 (3)1.0215 (3)0.9891 (3)0.060 (3)*0.5
H3S0.9091751.0431350.9832540.072*0.5
C4S0.9381 (4)0.9676 (3)0.9804 (4)0.077 (4)*0.5
H4S0.8990090.9529060.9688500.093*0.5
C5S0.9891 (5)0.9354 (2)0.9888 (4)0.096 (5)*0.5
H5S0.9850330.8986840.9829840.115*0.5
C6S1.0463 (5)0.9575 (3)1.0057 (5)0.103 (5)*0.5
H6S1.0813300.9357631.0113930.124*0.5
C7S1.0522 (3)1.0114 (3)1.0143 (4)0.105 (5)*0.5
H7S1.0913471.0259981.0257640.127*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ta10.01097 (6)0.01775 (7)0.01564 (6)0.00017 (5)0.00330 (5)0.00109 (5)
Ta20.01086 (6)0.01959 (7)0.01530 (7)0.00063 (5)0.00306 (5)0.00148 (5)
O10.0135 (10)0.0175 (11)0.0151 (11)0.0009 (8)0.0035 (8)0.0003 (9)
N10.0151 (13)0.0231 (15)0.0205 (14)0.0003 (11)0.0057 (11)0.0015 (12)
N20.0168 (13)0.0202 (15)0.0193 (14)0.0017 (11)0.0058 (11)0.0011 (11)
N30.0198 (15)0.0264 (17)0.0386 (18)0.0044 (12)0.0114 (13)0.0051 (14)
N40.0201 (15)0.0281 (17)0.0428 (19)0.0041 (12)0.0147 (14)0.0086 (14)
N50.0173 (14)0.0271 (16)0.0188 (14)0.0026 (11)0.0019 (11)0.0047 (12)
N60.0164 (13)0.0197 (14)0.0176 (14)0.0006 (11)0.0027 (11)0.0005 (11)
N70.0241 (15)0.0248 (16)0.0234 (15)0.0007 (12)0.0037 (12)0.0029 (12)
N80.0267 (16)0.0268 (16)0.0216 (15)0.0012 (13)0.0008 (12)0.0072 (13)
N90.0152 (13)0.0234 (15)0.0199 (14)0.0011 (11)0.0022 (11)0.0014 (12)
N100.0171 (13)0.0199 (14)0.0186 (14)0.0010 (11)0.0037 (11)0.0020 (11)
N110.0154 (14)0.0258 (16)0.0327 (17)0.0018 (12)0.0018 (12)0.0040 (13)
N120.0174 (14)0.0268 (17)0.0337 (17)0.0028 (12)0.0044 (12)0.0038 (13)
N130.0149 (13)0.0203 (15)0.0204 (14)0.0026 (11)0.0043 (11)0.0063 (11)
N140.0128 (13)0.0203 (15)0.0216 (14)0.0023 (11)0.0036 (11)0.0022 (11)
N150.0139 (13)0.0191 (14)0.0174 (13)0.0014 (10)0.0033 (10)0.0015 (11)
N160.0134 (13)0.0206 (15)0.0201 (14)0.0013 (11)0.0066 (11)0.0014 (11)
N170.0142 (13)0.0220 (15)0.0222 (14)0.0008 (11)0.0045 (11)0.0051 (12)
N180.0162 (13)0.0191 (14)0.0259 (15)0.0033 (11)0.0052 (11)0.0043 (12)
N190.0126 (13)0.0216 (15)0.0214 (14)0.0037 (11)0.0033 (11)0.0022 (11)
N200.0125 (13)0.0212 (15)0.0219 (14)0.0010 (11)0.0011 (11)0.0043 (12)
N210.0140 (13)0.0218 (15)0.0265 (15)0.0019 (11)0.0012 (11)0.0031 (12)
N220.0133 (13)0.0258 (15)0.0171 (14)0.0004 (11)0.0013 (11)0.0002 (11)
N230.0115 (13)0.0228 (15)0.0228 (14)0.0004 (11)0.0030 (11)0.0009 (12)
N240.0147 (14)0.0298 (17)0.0291 (16)0.0019 (12)0.0033 (12)0.0092 (13)
N250.0136 (14)0.0312 (17)0.0277 (16)0.0017 (12)0.0028 (12)0.0065 (13)
N260.0188 (14)0.0263 (16)0.0248 (15)0.0036 (12)0.0025 (12)0.0033 (13)
N270.0166 (13)0.0242 (15)0.0192 (14)0.0029 (11)0.0064 (11)0.0010 (12)
N280.0402 (19)0.0256 (17)0.0244 (16)0.0065 (14)0.0060 (14)0.0008 (13)
N290.0423 (19)0.0212 (16)0.0273 (17)0.0046 (14)0.0058 (14)0.0007 (13)
N300.0179 (14)0.0274 (16)0.0197 (14)0.0029 (12)0.0080 (11)0.0010 (12)
N310.0137 (13)0.0224 (15)0.0209 (14)0.0002 (11)0.0060 (11)0.0005 (12)
N320.0196 (14)0.0227 (16)0.0331 (17)0.0035 (12)0.0090 (13)0.0070 (13)
N330.0206 (15)0.0235 (16)0.0385 (18)0.0044 (12)0.0126 (13)0.0034 (14)
N340.0147 (13)0.0284 (16)0.0184 (14)0.0005 (11)0.0032 (11)0.0055 (12)
N350.0210 (15)0.0283 (17)0.0289 (16)0.0055 (12)0.0001 (12)0.0079 (13)
N360.0291 (17)0.0228 (17)0.0376 (19)0.0039 (13)0.0026 (14)0.0030 (14)
C10.0163 (16)0.0241 (18)0.0182 (16)0.0012 (13)0.0039 (13)0.0012 (13)
C20.0153 (16)0.0310 (19)0.0148 (16)0.0009 (13)0.0024 (12)0.0039 (14)
C30.0187 (16)0.0299 (19)0.0191 (17)0.0004 (14)0.0050 (13)0.0017 (14)
C40.0264 (19)0.028 (2)0.0258 (19)0.0044 (15)0.0050 (15)0.0045 (15)
C50.0206 (18)0.043 (2)0.0267 (19)0.0072 (16)0.0060 (15)0.0098 (17)
C60.0183 (17)0.043 (2)0.0243 (18)0.0039 (15)0.0075 (14)0.0080 (16)
C70.0174 (16)0.032 (2)0.0205 (17)0.0055 (14)0.0060 (13)0.0046 (15)
C80.0156 (16)0.0246 (18)0.0223 (17)0.0014 (13)0.0063 (13)0.0018 (14)
C90.0170 (16)0.0275 (19)0.0227 (17)0.0014 (13)0.0069 (13)0.0034 (14)
C100.0284 (19)0.029 (2)0.0243 (19)0.0020 (15)0.0067 (15)0.0038 (15)
C110.032 (2)0.039 (2)0.0181 (18)0.0048 (17)0.0043 (15)0.0019 (16)
C120.0283 (19)0.040 (2)0.0199 (18)0.0065 (16)0.0050 (15)0.0110 (16)
C130.034 (2)0.029 (2)0.033 (2)0.0008 (16)0.0035 (17)0.0119 (17)
C140.029 (2)0.031 (2)0.0257 (19)0.0025 (16)0.0005 (15)0.0042 (16)
C150.0161 (16)0.0258 (19)0.0202 (17)0.0013 (13)0.0044 (13)0.0030 (14)
C160.0180 (17)0.033 (2)0.0193 (17)0.0009 (14)0.0049 (13)0.0025 (15)
C170.0190 (17)0.032 (2)0.0288 (19)0.0016 (15)0.0024 (14)0.0028 (16)
C180.0157 (18)0.054 (3)0.038 (2)0.0057 (17)0.0014 (16)0.009 (2)
C190.0187 (19)0.058 (3)0.042 (2)0.0070 (18)0.0017 (17)0.005 (2)
C200.027 (2)0.037 (2)0.057 (3)0.0079 (18)0.0011 (19)0.001 (2)
C210.0210 (18)0.033 (2)0.041 (2)0.0008 (15)0.0014 (16)0.0032 (18)
C220.0270 (19)0.0230 (19)0.030 (2)0.0012 (15)0.0073 (15)0.0023 (15)
C230.0207 (17)0.0268 (19)0.0224 (18)0.0009 (14)0.0049 (14)0.0057 (15)
C240.0117 (15)0.0208 (17)0.0227 (17)0.0015 (12)0.0033 (13)0.0012 (13)
C250.0107 (14)0.0188 (17)0.0252 (17)0.0005 (12)0.0023 (13)0.0041 (13)
C260.0226 (17)0.0206 (17)0.0208 (17)0.0016 (13)0.0085 (14)0.0019 (14)
C270.0213 (17)0.0188 (17)0.0303 (19)0.0002 (13)0.0047 (14)0.0010 (14)
C280.0258 (19)0.0247 (19)0.036 (2)0.0051 (15)0.0094 (16)0.0087 (16)
C290.038 (2)0.038 (2)0.0243 (19)0.0088 (18)0.0079 (17)0.0085 (17)
C300.0273 (19)0.032 (2)0.0243 (19)0.0054 (15)0.0026 (15)0.0024 (16)
C310.0129 (15)0.0247 (18)0.0265 (18)0.0007 (13)0.0016 (13)0.0033 (14)
C320.0146 (16)0.0203 (18)0.035 (2)0.0022 (13)0.0023 (14)0.0037 (15)
C330.0232 (18)0.0223 (19)0.044 (2)0.0000 (14)0.0115 (16)0.0077 (17)
C340.0258 (19)0.022 (2)0.063 (3)0.0015 (15)0.0213 (19)0.0016 (19)
C350.0189 (19)0.027 (2)0.070 (3)0.0054 (15)0.0027 (19)0.002 (2)
C360.040 (2)0.036 (2)0.045 (3)0.0147 (19)0.011 (2)0.001 (2)
C370.032 (2)0.035 (2)0.036 (2)0.0088 (17)0.0013 (17)0.0007 (18)
C380.0141 (15)0.0203 (17)0.0194 (16)0.0011 (12)0.0042 (12)0.0041 (13)
C390.0150 (15)0.0205 (17)0.0202 (16)0.0001 (13)0.0037 (13)0.0036 (13)
C400.0174 (16)0.0264 (19)0.0235 (17)0.0017 (13)0.0044 (13)0.0011 (14)
C410.0151 (16)0.033 (2)0.034 (2)0.0046 (14)0.0066 (15)0.0013 (16)
C420.0154 (17)0.038 (2)0.038 (2)0.0034 (15)0.0052 (15)0.0055 (18)
C430.0248 (19)0.039 (2)0.028 (2)0.0001 (16)0.0008 (15)0.0110 (17)
C440.0183 (17)0.031 (2)0.0251 (18)0.0026 (14)0.0044 (14)0.0025 (15)
C450.0156 (15)0.0214 (18)0.0219 (17)0.0039 (13)0.0068 (13)0.0001 (13)
C460.0214 (17)0.0205 (17)0.0228 (17)0.0037 (13)0.0095 (14)0.0003 (14)
C470.048 (2)0.026 (2)0.029 (2)0.0104 (18)0.0011 (18)0.0016 (16)
C480.077 (3)0.034 (2)0.021 (2)0.009 (2)0.001 (2)0.0020 (17)
C490.055 (3)0.025 (2)0.029 (2)0.0017 (18)0.0143 (19)0.0052 (16)
C500.028 (2)0.023 (2)0.044 (2)0.0058 (15)0.0086 (17)0.0022 (17)
C510.0235 (18)0.027 (2)0.031 (2)0.0007 (15)0.0021 (15)0.0039 (16)
C520.0171 (15)0.0195 (16)0.0260 (17)0.0030 (12)0.0073 (13)0.0052 (13)
C530.016 (3)0.020 (4)0.022 (4)0.000 (3)0.008 (3)0.008 (3)
C540.016 (3)0.030 (4)0.019 (3)0.003 (3)0.008 (2)0.005 (3)
C550.025 (4)0.034 (4)0.023 (3)0.002 (3)0.008 (3)0.005 (3)
C560.022 (4)0.035 (4)0.032 (4)0.002 (3)0.015 (3)0.007 (3)
C570.018 (3)0.030 (4)0.041 (4)0.003 (3)0.012 (3)0.006 (3)
C580.025 (4)0.027 (4)0.038 (4)0.002 (3)0.005 (3)0.001 (3)
C53B0.017 (4)0.020 (4)0.023 (4)0.004 (3)0.005 (3)0.005 (3)
C54B0.015 (3)0.026 (4)0.026 (4)0.004 (3)0.005 (3)0.007 (3)
C55B0.026 (4)0.033 (4)0.022 (3)0.001 (3)0.007 (3)0.002 (3)
C56B0.022 (4)0.037 (4)0.030 (4)0.000 (3)0.009 (3)0.006 (3)
C57B0.020 (4)0.041 (4)0.035 (4)0.003 (3)0.004 (3)0.005 (3)
C58B0.017 (3)0.024 (4)0.027 (4)0.002 (3)0.007 (3)0.006 (3)
C590.0250 (18)0.034 (2)0.0232 (18)0.0006 (15)0.0053 (15)0.0121 (16)
C600.0232 (18)0.036 (2)0.0162 (17)0.0011 (15)0.0054 (14)0.0038 (15)
C610.0253 (19)0.029 (2)0.045 (2)0.0055 (16)0.0090 (17)0.0051 (18)
C620.029 (2)0.033 (2)0.053 (3)0.0013 (17)0.0161 (19)0.0060 (19)
C630.037 (2)0.036 (2)0.065 (3)0.0051 (19)0.022 (2)0.007 (2)
C640.037 (2)0.032 (2)0.042 (2)0.0052 (18)0.0095 (19)0.0071 (18)
Ta1A0.01206 (6)0.01466 (7)0.01334 (6)0.00030 (5)0.00184 (5)0.00029 (5)
Ta2A0.01178 (6)0.01450 (7)0.01351 (6)0.00023 (5)0.00254 (5)0.00019 (5)
O1A0.0135 (10)0.0173 (11)0.0117 (10)0.0019 (8)0.0021 (8)0.0012 (9)
N1A0.0155 (13)0.0216 (15)0.0176 (14)0.0024 (11)0.0021 (11)0.0005 (11)
N2A0.0170 (14)0.0193 (15)0.0205 (14)0.0005 (11)0.0032 (11)0.0050 (11)
N3A0.0180 (15)0.0305 (17)0.0321 (17)0.0008 (12)0.0001 (13)0.0079 (14)
N4A0.0174 (15)0.0339 (18)0.0365 (18)0.0043 (13)0.0020 (13)0.0088 (14)
N5A0.0185 (14)0.0214 (15)0.0180 (14)0.0000 (11)0.0032 (11)0.0026 (11)
N6A0.0192 (14)0.0190 (15)0.0191 (14)0.0000 (11)0.0035 (11)0.0006 (11)
N7A0.0304 (17)0.0234 (16)0.0275 (16)0.0005 (13)0.0005 (13)0.0012 (13)
N8A0.0364 (18)0.0215 (16)0.0265 (16)0.0008 (13)0.0010 (14)0.0045 (13)
N9A0.0152 (13)0.0203 (14)0.0179 (14)0.0003 (11)0.0050 (11)0.0009 (11)
N10A0.0185 (14)0.0170 (14)0.0155 (13)0.0013 (11)0.0054 (11)0.0001 (11)
N11A0.0216 (15)0.0221 (16)0.0311 (17)0.0046 (12)0.0108 (13)0.0064 (13)
N12A0.0196 (15)0.0255 (16)0.0319 (17)0.0062 (12)0.0114 (13)0.0048 (13)
N13A0.0139 (13)0.0176 (14)0.0168 (13)0.0009 (10)0.0026 (10)0.0039 (11)
N18A0.0156 (13)0.0184 (14)0.0202 (14)0.0013 (11)0.0040 (11)0.0002 (11)
N19A0.0125 (12)0.0182 (14)0.0182 (14)0.0013 (10)0.0027 (10)0.0001 (11)
N20A0.0147 (13)0.0164 (14)0.0191 (14)0.0012 (10)0.0033 (11)0.0011 (11)
N21A0.0185 (14)0.0177 (14)0.0233 (15)0.0029 (11)0.0087 (11)0.0007 (11)
N14A0.0167 (13)0.0164 (14)0.0185 (14)0.0030 (10)0.0053 (11)0.0012 (11)
N15A0.0140 (13)0.0168 (14)0.0155 (13)0.0010 (10)0.0039 (10)0.0017 (11)
N16A0.0132 (13)0.0172 (14)0.0196 (14)0.0014 (10)0.0039 (11)0.0003 (11)
N17A0.0168 (13)0.0165 (14)0.0203 (14)0.0029 (11)0.0015 (11)0.0014 (11)
N22A0.0161 (13)0.0229 (15)0.0174 (14)0.0014 (11)0.0049 (11)0.0014 (11)
N23A0.0162 (13)0.0185 (14)0.0194 (14)0.0001 (11)0.0056 (11)0.0019 (11)
N24A0.0187 (15)0.0352 (18)0.0380 (18)0.0060 (13)0.0113 (13)0.0153 (15)
N25A0.0183 (15)0.0373 (19)0.0398 (19)0.0058 (13)0.0137 (14)0.0154 (15)
N26A0.0212 (14)0.0185 (15)0.0192 (14)0.0009 (11)0.0047 (11)0.0029 (11)
N27A0.0151 (13)0.0207 (15)0.0174 (14)0.0014 (11)0.0012 (11)0.0028 (11)
N28A0.0241 (15)0.0215 (16)0.0262 (16)0.0012 (12)0.0035 (12)0.0008 (12)
N29A0.0249 (15)0.0187 (15)0.0290 (16)0.0019 (12)0.0009 (13)0.0014 (12)
N30A0.0150 (13)0.0186 (14)0.0185 (14)0.0015 (10)0.0031 (11)0.0022 (11)
N31A0.0129 (13)0.0157 (14)0.0171 (13)0.0007 (10)0.0012 (10)0.0000 (11)
N32A0.0169 (14)0.0264 (16)0.0246 (15)0.0022 (12)0.0040 (12)0.0064 (12)
N33A0.0145 (14)0.0273 (16)0.0284 (16)0.0036 (12)0.0023 (12)0.0034 (13)
N34A0.0170 (13)0.0174 (14)0.0163 (13)0.0022 (11)0.0021 (10)0.0022 (11)
N35A0.0195 (14)0.0224 (15)0.0263 (16)0.0060 (12)0.0019 (12)0.0018 (12)
N36A0.0268 (16)0.0245 (16)0.0250 (16)0.0057 (12)0.0020 (13)0.0035 (13)
C1A0.0157 (16)0.0198 (17)0.0243 (17)0.0002 (13)0.0022 (13)0.0005 (14)
C2A0.0180 (16)0.0194 (17)0.0230 (17)0.0026 (13)0.0006 (13)0.0055 (14)
C3A0.0218 (17)0.0223 (18)0.0261 (18)0.0044 (14)0.0025 (14)0.0043 (14)
C4A0.031 (2)0.027 (2)0.0236 (18)0.0091 (15)0.0005 (15)0.0010 (15)
C5A0.0250 (19)0.026 (2)0.034 (2)0.0092 (15)0.0127 (16)0.0083 (16)
C6A0.0163 (17)0.028 (2)0.049 (2)0.0006 (15)0.0046 (16)0.0054 (18)
C7A0.0195 (17)0.0253 (19)0.034 (2)0.0006 (14)0.0005 (15)0.0009 (16)
C8A0.0174 (16)0.0232 (18)0.0217 (17)0.0004 (13)0.0020 (13)0.0029 (14)
C9A0.0180 (16)0.0270 (19)0.0254 (18)0.0032 (14)0.0021 (14)0.0071 (15)
C10A0.0141 (16)0.0265 (19)0.0280 (19)0.0023 (13)0.0037 (14)0.0055 (15)
C11A0.0204 (18)0.045 (2)0.0234 (19)0.0051 (16)0.0031 (14)0.0065 (17)
C12A0.030 (2)0.043 (2)0.026 (2)0.0045 (17)0.0020 (16)0.0150 (18)
C13A0.052 (3)0.026 (2)0.039 (2)0.0001 (19)0.005 (2)0.0108 (18)
C14A0.050 (3)0.026 (2)0.027 (2)0.0003 (18)0.0011 (18)0.0029 (16)
C15A0.0157 (15)0.0236 (18)0.0153 (15)0.0018 (13)0.0018 (12)0.0019 (13)
C16A0.0169 (16)0.0295 (19)0.0151 (16)0.0015 (13)0.0032 (13)0.0017 (14)
C17A0.0245 (18)0.027 (2)0.034 (2)0.0002 (15)0.0101 (16)0.0001 (16)
C18A0.0206 (18)0.040 (2)0.038 (2)0.0050 (16)0.0133 (16)0.0044 (18)
C19A0.0219 (18)0.041 (2)0.036 (2)0.0058 (16)0.0146 (16)0.0040 (18)
C20A0.037 (2)0.031 (2)0.051 (3)0.0043 (17)0.022 (2)0.0018 (19)
C21A0.0254 (19)0.029 (2)0.038 (2)0.0013 (15)0.0161 (16)0.0010 (17)
C22A0.0242 (18)0.0224 (18)0.0226 (17)0.0042 (14)0.0063 (14)0.0029 (14)
C23A0.0218 (17)0.0225 (18)0.0177 (16)0.0011 (13)0.0018 (13)0.0037 (13)
C31A0.0163 (16)0.0190 (17)0.0203 (16)0.0009 (13)0.0031 (13)0.0015 (13)
C32A0.0192 (16)0.0170 (17)0.0261 (18)0.0001 (13)0.0085 (14)0.0010 (14)
C33A0.0204 (17)0.0179 (17)0.0295 (19)0.0006 (13)0.0054 (14)0.0009 (14)
C34A0.0191 (17)0.0221 (18)0.035 (2)0.0010 (14)0.0014 (15)0.0029 (15)
C35A0.0208 (18)0.0191 (18)0.048 (2)0.0050 (14)0.0136 (16)0.0018 (16)
C36A0.041 (2)0.035 (2)0.034 (2)0.0132 (18)0.0136 (18)0.0042 (18)
C37A0.037 (2)0.034 (2)0.028 (2)0.0149 (17)0.0060 (17)0.0006 (17)
C24A0.0153 (15)0.0204 (17)0.0175 (16)0.0003 (12)0.0032 (12)0.0012 (13)
C25A0.0175 (16)0.0199 (17)0.0206 (17)0.0033 (13)0.0012 (13)0.0007 (13)
C30A0.052 (3)0.028 (2)0.0219 (19)0.0158 (18)0.0056 (17)0.0024 (16)
C29A0.061 (3)0.030 (2)0.023 (2)0.019 (2)0.0030 (19)0.0030 (17)
C28A0.0253 (19)0.0195 (18)0.039 (2)0.0077 (14)0.0067 (16)0.0046 (16)
C27A0.0173 (16)0.0229 (18)0.032 (2)0.0004 (13)0.0047 (14)0.0058 (15)
C26A0.0165 (16)0.0224 (18)0.0230 (17)0.0012 (13)0.0049 (13)0.0004 (14)
C38A0.0186 (16)0.0184 (17)0.0210 (17)0.0039 (13)0.0053 (13)0.0010 (13)
C39A0.0160 (16)0.0298 (19)0.0223 (17)0.0060 (14)0.0075 (13)0.0052 (15)
C40A0.0232 (18)0.031 (2)0.039 (2)0.0012 (15)0.0127 (16)0.0012 (17)
C41A0.025 (2)0.048 (3)0.051 (3)0.0014 (18)0.0217 (19)0.001 (2)
C42A0.030 (2)0.061 (3)0.032 (2)0.006 (2)0.0177 (17)0.005 (2)
C43A0.028 (2)0.052 (3)0.028 (2)0.0056 (18)0.0070 (16)0.0097 (18)
C44A0.0180 (17)0.036 (2)0.0256 (19)0.0022 (15)0.0043 (14)0.0023 (16)
C45A0.0146 (15)0.0179 (17)0.0191 (16)0.0000 (12)0.0059 (12)0.0001 (13)
C46A0.0169 (16)0.0201 (17)0.0216 (17)0.0018 (13)0.0075 (13)0.0012 (13)
C51A0.0241 (18)0.0231 (19)0.0273 (19)0.0021 (14)0.0009 (15)0.0004 (15)
C50A0.040 (2)0.0177 (19)0.039 (2)0.0015 (16)0.0004 (18)0.0018 (16)
C49A0.045 (2)0.025 (2)0.027 (2)0.0055 (17)0.0011 (17)0.0093 (16)
C48A0.041 (2)0.032 (2)0.0241 (19)0.0028 (17)0.0016 (17)0.0008 (16)
C47A0.033 (2)0.0195 (18)0.0241 (18)0.0022 (15)0.0035 (15)0.0018 (14)
C52A0.0173 (16)0.0184 (17)0.0191 (16)0.0020 (12)0.0050 (13)0.0030 (13)
C53A0.0145 (16)0.0231 (18)0.0222 (17)0.0029 (13)0.0039 (13)0.0070 (14)
C58A0.0190 (17)0.034 (2)0.0266 (19)0.0005 (15)0.0030 (14)0.0000 (16)
C57A0.0190 (18)0.042 (2)0.042 (2)0.0050 (16)0.0040 (16)0.0070 (19)
C56A0.0148 (17)0.046 (2)0.035 (2)0.0058 (16)0.0034 (15)0.0085 (18)
C55A0.0238 (19)0.037 (2)0.027 (2)0.0098 (16)0.0015 (15)0.0023 (16)
C54A0.0187 (17)0.0268 (19)0.0279 (19)0.0044 (14)0.0043 (14)0.0049 (15)
C59A0.0297 (19)0.0217 (18)0.0236 (18)0.0002 (14)0.0054 (15)0.0047 (14)
C60A0.0247 (17)0.0223 (18)0.0129 (15)0.0017 (13)0.0039 (13)0.0012 (13)
C61A0.0210 (18)0.032 (2)0.0292 (19)0.0041 (15)0.0028 (15)0.0056 (16)
C62A0.0205 (19)0.033 (2)0.059 (3)0.0019 (16)0.0059 (18)0.009 (2)
C63A0.029 (2)0.037 (2)0.044 (2)0.0023 (17)0.0137 (18)0.0044 (19)
C64A0.0247 (18)0.0238 (19)0.034 (2)0.0031 (14)0.0037 (15)0.0020 (16)
Geometric parameters (Å, º) top
Ta1—O11.938 (2)Ta1A—N6A2.210 (3)
Ta1—N22.204 (3)Ta1A—N10A2.211 (3)
Ta1—N62.202 (3)Ta1A—N13A1.929 (3)
Ta1—N102.213 (3)Ta1A—N19A2.280 (3)
Ta1—N131.924 (3)Ta1A—N15A2.249 (3)
Ta1—N152.265 (3)Ta2A—O1A1.932 (2)
Ta1—N192.283 (3)Ta2A—N20A2.269 (3)
Ta2—O11.921 (2)Ta2A—N16A2.273 (3)
Ta2—N162.280 (3)Ta2A—N23A2.217 (3)
Ta2—N202.281 (3)Ta2A—N27A2.215 (3)
Ta2—N232.204 (3)Ta2A—N31A2.211 (3)
Ta2—N272.218 (3)Ta2A—N34A1.928 (3)
Ta2—N312.194 (3)N1A—N2A1.332 (4)
Ta2—N341.928 (3)N1A—C1A1.332 (4)
N1—N21.346 (4)N2A—N3A1.326 (4)
N1—C11.330 (4)N3A—N4A1.329 (4)
N2—N31.334 (4)N4A—C1A1.347 (5)
N3—N41.328 (4)N5A—N6A1.340 (4)
N4—C11.344 (5)N5A—C8A1.326 (4)
N5—N61.339 (4)N6A—N7A1.322 (4)
N5—C81.337 (5)N7A—N8A1.339 (4)
N6—N71.327 (4)N8A—C8A1.345 (5)
N7—N81.337 (4)N9A—N10A1.352 (4)
N8—C81.343 (5)N9A—C15A1.332 (4)
N9—N101.342 (4)N10A—N11A1.329 (4)
N9—C151.337 (4)N11A—N12A1.326 (4)
N10—N111.327 (4)N12A—C15A1.345 (5)
N11—N121.319 (4)N13A—C22A1.447 (4)
N12—C151.344 (5)N13A—C23A1.474 (4)
N13—C221.450 (5)N18A—N19A1.324 (4)
N13—C231.473 (4)N18A—C31A1.339 (4)
N14—N151.321 (4)N19A—N20A1.328 (4)
N14—C241.340 (4)N20A—N21A1.331 (4)
N15—N161.329 (4)N21A—C31A1.345 (4)
N16—N171.330 (4)N14A—N15A1.328 (4)
N17—C241.350 (4)N14A—C24A1.336 (4)
N18—N191.323 (4)N15A—N16A1.334 (4)
N18—C311.339 (4)N16A—N17A1.324 (4)
N19—N201.328 (4)N17A—C24A1.351 (4)
N20—N211.328 (4)N22A—N23A1.336 (4)
N21—C311.345 (5)N22A—C38A1.325 (4)
N22—N231.339 (4)N23A—N24A1.333 (4)
N22—C381.331 (4)N24A—N25A1.329 (4)
N23—N241.322 (4)N25A—C38A1.351 (5)
N24—N251.322 (4)N26A—N27A1.351 (4)
N25—C381.354 (4)N26A—C45A1.331 (4)
N26—N271.345 (4)N27A—N28A1.329 (4)
N26—C451.332 (4)N28A—N29A1.327 (4)
N27—N281.329 (4)N29A—C45A1.349 (4)
N28—N291.330 (4)N30A—N31A1.343 (4)
N29—C451.344 (5)N30A—C52A1.339 (4)
N30—N311.337 (4)N31A—N32A1.330 (4)
N30—C521.331 (4)N32A—N33A1.322 (4)
N31—N321.328 (4)N33A—C52A1.348 (4)
N32—N331.328 (4)N34A—C59A1.455 (4)
N33—C521.343 (5)N34A—C60A1.469 (4)
N34—C591.458 (5)N35A—H35D0.9100
N34—C601.464 (5)N35A—H35E0.9100
N35—H35B0.9100N35A—C61A1.475 (4)
N35—H35C0.9100N35A—C62A1.477 (5)
N35—C611.488 (5)N36A—H36D0.9100
N35—C621.476 (5)N36A—H36E0.9100
N36—H36B0.9100N36A—C63A1.478 (5)
N36—H36C0.9100N36A—C64A1.484 (5)
N36—C631.475 (5)C1A—C2A1.472 (5)
N36—C641.480 (5)C2A—C3A1.390 (5)
C1—C21.477 (5)C2A—C7A1.398 (5)
C2—C31.386 (5)C3A—H3A0.9500
C2—C71.398 (5)C3A—C4A1.389 (5)
C3—H30.9500C4A—H4A0.9500
C3—C41.380 (5)C4A—C5A1.390 (6)
C4—H40.9500C5A—H5A0.9500
C4—C51.388 (5)C5A—C6A1.374 (6)
C5—H50.9500C6A—H6A0.9500
C5—C61.384 (6)C6A—C7A1.389 (5)
C6—H60.9500C7A—H7A0.9500
C6—C71.392 (5)C8A—C9A1.475 (5)
C7—H70.9500C9A—C10A1.389 (5)
C8—C91.468 (5)C9A—C14A1.392 (5)
C9—C101.387 (5)C10A—H10A0.9500
C9—C141.388 (5)C10A—C11A1.389 (5)
C10—H100.9500C11A—H11A0.9500
C10—C111.387 (5)C11A—C12A1.381 (6)
C11—H110.9500C12A—H12A0.9500
C11—C121.376 (6)C12A—C13A1.380 (6)
C12—H120.9500C13A—H13A0.9500
C12—C131.381 (6)C13A—C14A1.391 (5)
C13—H130.9500C14A—H14A0.9500
C13—C141.388 (5)C15A—C16A1.479 (5)
C14—H140.9500C16A—C17A1.393 (5)
C15—C161.471 (5)C16A—C21A1.382 (5)
C16—C171.403 (5)C17A—H17A0.9500
C16—C211.385 (5)C17A—C18A1.390 (5)
C17—H170.9500C18A—H18A0.9500
C17—C181.382 (5)C18A—C19A1.377 (6)
C18—H180.9500C19A—H19A0.9500
C18—C191.383 (6)C19A—C20A1.379 (6)
C19—H190.9500C20A—H20A0.9500
C19—C201.380 (6)C20A—C21A1.395 (5)
C20—H200.9500C21A—H21A0.9500
C20—C211.386 (5)C22A—H22D0.9800
C21—H210.9500C22A—H22E0.9800
C22—H22A0.9800C22A—H22F0.9800
C22—H22B0.9800C23A—H23D0.9800
C22—H22C0.9800C23A—H23E0.9800
C23—H23A0.9800C23A—H23F0.9800
C23—H23B0.9800C31A—C32A1.468 (5)
C23—H23C0.9800C32A—C33A1.385 (5)
C24—C251.472 (4)C32A—C37A1.394 (5)
C25—C261.389 (5)C33A—H33A0.9500
C25—C301.392 (5)C33A—C34A1.392 (5)
C26—H260.9500C34A—H34A0.9500
C26—C271.381 (5)C34A—C35A1.383 (5)
C27—H270.9500C35A—H35A0.9500
C27—C281.386 (5)C35A—C36A1.372 (6)
C28—H280.9500C36A—H36A0.9500
C28—C291.380 (6)C36A—C37A1.389 (5)
C29—H290.9500C37A—H37A0.9500
C29—C301.393 (5)C24A—C25A1.468 (5)
C30—H300.9500C25A—C30A1.389 (5)
C31—C321.472 (5)C25A—C26A1.393 (5)
C32—C331.384 (5)C30A—H30A0.9500
C32—C371.393 (5)C30A—C29A1.385 (5)
C33—H330.9500C29A—H29A0.9500
C33—C341.391 (5)C29A—C28A1.385 (6)
C34—H340.9500C28A—H28A0.9500
C34—C351.373 (6)C28A—C27A1.384 (5)
C35—H350.9500C27A—H27A0.9500
C35—C361.386 (7)C27A—C26A1.382 (5)
C36—H360.9500C26A—H26A0.9500
C36—C371.387 (5)C38A—C39A1.474 (5)
C37—H370.9500C39A—C40A1.394 (5)
C38—C391.471 (4)C39A—C44A1.391 (5)
C39—C401.400 (5)C40A—H40A0.9500
C39—C441.386 (5)C40A—C41A1.396 (5)
C40—H400.9500C41A—H41A0.9500
C40—C411.383 (5)C41A—C42A1.383 (6)
C41—H410.9500C42A—H42A0.9500
C41—C421.380 (5)C42A—C43A1.379 (6)
C42—H420.9500C43A—H43A0.9500
C42—C431.389 (5)C43A—C44A1.390 (5)
C43—H430.9500C44A—H44A0.9500
C43—C441.384 (5)C45A—C46A1.470 (5)
C44—H440.9500C46A—C51A1.390 (5)
C45—C461.476 (5)C46A—C47A1.388 (5)
C46—C471.381 (5)C51A—H51A0.9500
C46—C511.397 (5)C51A—C50A1.386 (5)
C47—H470.9500C50A—H50A0.9500
C47—C481.390 (6)C50A—C49A1.380 (6)
C48—H480.9500C49A—H49A0.9500
C48—C491.376 (6)C49A—C48A1.382 (6)
C49—H490.9500C48A—H48A0.9500
C49—C501.381 (6)C48A—C47A1.384 (5)
C50—H500.9500C47A—H47A0.9500
C50—C511.382 (5)C52A—C53A1.475 (4)
C51—H510.9500C53A—C58A1.399 (5)
C52—C531.482 (4)C53A—C54A1.390 (5)
C52—C53B1.478 (4)C58A—H58A0.9500
C53—C541.3900C58A—C57A1.382 (5)
C53—C581.3900C57A—H57A0.9500
C54—H540.9500C57A—C56A1.386 (6)
C54—C551.3900C56A—H56A0.9500
C55—H550.9500C56A—C55A1.391 (6)
C55—C561.3900C55A—H55A0.9500
C56—H560.9500C55A—C54A1.394 (5)
C56—C571.3900C54A—H54A0.9500
C57—H570.9500C59A—H59D0.9800
C57—C581.3900C59A—H59E0.9800
C58—H580.9500C59A—H59F0.9800
C53B—C54B1.3900C60A—H60D0.9800
C53B—C58B1.3900C60A—H60E0.9800
C54B—H54B0.9500C60A—H60F0.9800
C54B—C55B1.3900C61A—H61D0.9800
C55B—H55B0.9500C61A—H61E0.9800
C55B—C56B1.3900C61A—H61F0.9800
C56B—H56B0.9500C62A—H62D0.9800
C56B—C57B1.3900C62A—H62E0.9800
C57B—H57B0.9500C62A—H62F0.9800
C57B—C58B1.3900C63A—H63D0.9800
C58B—H58B0.9500C63A—H63E0.9800
C59—H59A0.9800C63A—H63F0.9800
C59—H59B0.9800C64A—H64D0.9800
C59—H59C0.9800C64A—H64E0.9800
C60—H60A0.9800C64A—H64F0.9800
C60—H60B0.9800C1S—H1SA0.9800
C60—H60C0.9800C1S—H1SB0.9800
C61—H61A0.9800C1S—H1SC0.9800
C61—H61B0.9800C1S—C2S1.5076
C61—H61C0.9800C2S—C3S1.4025
C62—H62A0.9800C2S—C7S1.4023
C62—H62B0.9800C3S—H3S0.9500
C62—H62C0.9800C3S—C4S1.3964
C63—H63A0.9800C4S—H4S0.9500
C63—H63B0.9800C4S—C5S1.3961
C63—H63C0.9800C5S—H5S0.9500
C64—H64A0.9800C5S—C6S1.3967
C64—H64B0.9800C6S—H6S0.9500
C64—H64C0.9800C6S—C7S1.3962
Ta1A—O1A1.932 (2)C7S—H7S0.9500
Ta1A—N2A2.204 (3)
O1—Ta1—N2101.48 (9)O1A—Ta1A—N10A101.30 (9)
O1—Ta1—N688.21 (10)O1A—Ta1A—N19A73.56 (9)
O1—Ta1—N10100.35 (10)O1A—Ta1A—N15A74.54 (9)
O1—Ta1—N1573.91 (9)N2A—Ta1A—N6A72.38 (10)
O1—Ta1—N1974.19 (9)N2A—Ta1A—N10A138.48 (10)
N2—Ta1—N10138.26 (10)N2A—Ta1A—N19A74.32 (10)
N2—Ta1—N15145.54 (10)N2A—Ta1A—N15A146.34 (10)
N2—Ta1—N1973.53 (10)N6A—Ta1A—N10A74.19 (10)
N6—Ta1—N272.55 (10)N6A—Ta1A—N19A137.55 (10)
N6—Ta1—N1073.05 (10)N6A—Ta1A—N15A139.30 (10)
N6—Ta1—N15139.68 (10)N10A—Ta1A—N19A145.96 (10)
N6—Ta1—N19137.46 (10)N10A—Ta1A—N15A73.71 (10)
N10—Ta1—N1575.06 (10)N13A—Ta1A—O1A151.05 (10)
N10—Ta1—N19147.23 (10)N13A—Ta1A—N2A87.48 (11)
N13—Ta1—O1150.60 (11)N13A—Ta1A—N6A120.93 (11)
N13—Ta1—N288.46 (11)N13A—Ta1A—N10A89.13 (10)
N13—Ta1—N6121.19 (11)N13A—Ta1A—N19A82.66 (11)
N13—Ta1—N1089.62 (11)N13A—Ta1A—N15A82.82 (10)
N13—Ta1—N1582.25 (11)N15A—Ta1A—N19A72.51 (9)
N13—Ta1—N1982.46 (11)O1A—Ta2A—N20A73.75 (9)
N15—Ta1—N1972.39 (10)O1A—Ta2A—N16A74.50 (9)
O1—Ta2—N1674.62 (9)O1A—Ta2A—N23A101.46 (9)
O1—Ta2—N2073.95 (9)O1A—Ta2A—N27A89.05 (9)
O1—Ta2—N2399.41 (10)O1A—Ta2A—N31A97.12 (9)
O1—Ta2—N2789.39 (10)N20A—Ta2A—N16A71.02 (9)
O1—Ta2—N31100.74 (10)N23A—Ta2A—N20A72.16 (10)
O1—Ta2—N34151.45 (11)N23A—Ta2A—N16A142.55 (10)
N16—Ta2—N2072.06 (9)N27A—Ta2A—N20A137.39 (10)
N23—Ta2—N16145.21 (10)N27A—Ta2A—N16A141.90 (10)
N23—Ta2—N2073.37 (10)N27A—Ta2A—N23A73.66 (10)
N23—Ta2—N2774.12 (10)N31A—Ta2A—N20A146.12 (10)
N27—Ta2—N16138.60 (10)N31A—Ta2A—N16A75.10 (10)
N27—Ta2—N20140.16 (10)N31A—Ta2A—N23A141.41 (10)
N31—Ta2—N1673.54 (10)N31A—Ta2A—N27A73.15 (10)
N31—Ta2—N20145.35 (10)N34A—Ta2A—O1A151.80 (10)
N31—Ta2—N23140.38 (10)N34A—Ta2A—N20A83.89 (11)
N31—Ta2—N2772.37 (10)N34A—Ta2A—N16A82.19 (11)
N34—Ta2—N1683.62 (11)N34A—Ta2A—N23A87.41 (11)
N34—Ta2—N2081.97 (11)N34A—Ta2A—N27A119.15 (11)
N34—Ta2—N2387.92 (11)N34A—Ta2A—N31A91.91 (11)
N34—Ta2—N27119.12 (11)Ta1A—O1A—Ta2A141.38 (12)
N34—Ta2—N3190.32 (11)C1A—N1A—N2A103.6 (3)
Ta2—O1—Ta1141.47 (12)N1A—N2A—Ta1A125.3 (2)
C1—N1—N2102.7 (3)N3A—N2A—Ta1A123.4 (2)
N1—N2—Ta1124.0 (2)N3A—N2A—N1A111.2 (3)
N3—N2—Ta1123.1 (2)N2A—N3A—N4A108.1 (3)
N3—N2—N1111.5 (3)N3A—N4A—C1A105.1 (3)
N4—N3—N2107.5 (3)C8A—N5A—N6A103.7 (3)
N3—N4—C1105.6 (3)N5A—N6A—Ta1A127.1 (2)
C8—N5—N6103.6 (3)N7A—N6A—Ta1A121.8 (2)
N5—N6—Ta1125.3 (2)N7A—N6A—N5A111.0 (3)
N7—N6—Ta1123.5 (2)N6A—N7A—N8A108.1 (3)
N7—N6—N5111.1 (3)N7A—N8A—C8A104.9 (3)
N6—N7—N8108.0 (3)C15A—N9A—N10A103.1 (3)
N7—N8—C8105.3 (3)N9A—N10A—Ta1A125.8 (2)
C15—N9—N10103.1 (3)N11A—N10A—Ta1A122.9 (2)
N9—N10—Ta1125.4 (2)N11A—N10A—N9A110.9 (3)
N11—N10—Ta1123.9 (2)N12A—N11A—N10A108.1 (3)
N11—N10—N9110.8 (3)N11A—N12A—C15A105.6 (3)
N12—N11—N10108.7 (3)C22A—N13A—Ta1A143.6 (2)
N11—N12—C15105.3 (3)C22A—N13A—C23A112.8 (3)
C22—N13—Ta1143.6 (2)C23A—N13A—Ta1A103.6 (2)
C22—N13—C23112.9 (3)N19A—N18A—C31A103.7 (3)
C23—N13—Ta1103.4 (2)N18A—N19A—Ta1A129.5 (2)
N15—N14—C24104.3 (3)N18A—N19A—N20A110.4 (3)
N14—N15—Ta1127.8 (2)N20A—N19A—Ta1A120.06 (19)
N14—N15—N16110.0 (3)N19A—N20A—Ta2A121.2 (2)
N16—N15—Ta1121.5 (2)N19A—N20A—N21A109.5 (3)
N15—N16—Ta2119.6 (2)N21A—N20A—Ta2A129.3 (2)
N15—N16—N17109.8 (3)N20A—N21A—C31A103.7 (3)
N17—N16—Ta2130.4 (2)N15A—N14A—C24A104.5 (3)
N16—N17—C24103.7 (3)N14A—N15A—Ta1A128.1 (2)
N19—N18—C31104.3 (3)N14A—N15A—N16A109.4 (2)
N18—N19—Ta1130.1 (2)N16A—N15A—Ta1A121.48 (19)
N18—N19—N20109.8 (3)N15A—N16A—Ta2A120.03 (19)
N20—N19—Ta1120.2 (2)N17A—N16A—Ta2A129.0 (2)
N19—N20—Ta2120.8 (2)N17A—N16A—N15A110.1 (3)
N21—N20—Ta2129.3 (2)N16A—N17A—C24A103.8 (3)
N21—N20—N19109.9 (3)C38A—N22A—N23A103.8 (3)
N20—N21—C31103.7 (3)N22A—N23A—Ta2A123.8 (2)
C38—N22—N23103.1 (3)N24A—N23A—Ta2A124.1 (2)
N22—N23—Ta2124.7 (2)N24A—N23A—N22A111.2 (3)
N24—N23—Ta2122.5 (2)N25A—N24A—N23A107.6 (3)
N24—N23—N22111.4 (3)N24A—N25A—C38A105.5 (3)
N23—N24—N25108.3 (3)C45A—N26A—N27A104.0 (3)
N24—N25—C38105.1 (3)N26A—N27A—Ta2A127.4 (2)
C45—N26—N27103.8 (3)N28A—N27A—Ta2A122.5 (2)
N26—N27—Ta2124.5 (2)N28A—N27A—N26A110.0 (3)
N28—N27—Ta2122.9 (2)N29A—N28A—N27A108.7 (3)
N28—N27—N26110.4 (3)N28A—N29A—C45A105.5 (3)
N27—N28—N29108.5 (3)C52A—N30A—N31A103.2 (3)
N28—N29—C45105.3 (3)N30A—N31A—Ta2A127.5 (2)
C52—N30—N31103.0 (3)N32A—N31A—Ta2A121.6 (2)
N30—N31—Ta2125.0 (2)N32A—N31A—N30A110.8 (3)
N32—N31—Ta2123.0 (2)N33A—N32A—N31A108.5 (3)
N32—N31—N30111.7 (3)N32A—N33A—C52A105.3 (3)
N31—N32—N33107.4 (3)C59A—N34A—Ta2A144.4 (2)
N32—N33—C52105.7 (3)C59A—N34A—C60A112.5 (3)
C59—N34—Ta2142.0 (2)C60A—N34A—Ta2A103.0 (2)
C59—N34—C60112.8 (3)H35D—N35A—H35E107.7
C60—N34—Ta2105.0 (2)C61A—N35A—H35D108.9
H35B—N35—H35C107.8C61A—N35A—H35E108.9
C61—N35—H35B109.0C61A—N35A—C62A113.2 (3)
C61—N35—H35C109.0C62A—N35A—H35D108.9
C62—N35—H35B109.0C62A—N35A—H35E108.9
C62—N35—H35C109.0H36D—N36A—H36E107.8
C62—N35—C61112.8 (3)C63A—N36A—H36D108.9
H36B—N36—H36C107.7C63A—N36A—H36E108.9
C63—N36—H36B108.8C63A—N36A—C64A113.1 (3)
C63—N36—H36C108.8C64A—N36A—H36D108.9
C63—N36—C64113.9 (3)C64A—N36A—H36E108.9
C64—N36—H36B108.8N1A—C1A—N4A112.0 (3)
C64—N36—H36C108.8N1A—C1A—C2A124.7 (3)
N1—C1—N4112.7 (3)N4A—C1A—C2A123.2 (3)
N1—C1—C2123.4 (3)C3A—C2A—C1A120.9 (3)
N4—C1—C2123.7 (3)C3A—C2A—C7A119.7 (3)
C3—C2—C1120.0 (3)C7A—C2A—C1A119.4 (3)
C3—C2—C7119.9 (3)C2A—C3A—H3A119.9
C7—C2—C1120.0 (3)C4A—C3A—C2A120.1 (3)
C2—C3—H3119.7C4A—C3A—H3A119.9
C4—C3—C2120.7 (3)C3A—C4A—H4A120.1
C4—C3—H3119.7C3A—C4A—C5A119.7 (4)
C3—C4—H4120.1C5A—C4A—H4A120.1
C3—C4—C5119.8 (4)C4A—C5A—H5A119.8
C5—C4—H4120.1C6A—C5A—C4A120.4 (3)
C4—C5—H5120.0C6A—C5A—H5A119.8
C6—C5—C4120.0 (3)C5A—C6A—H6A119.8
C6—C5—H5120.0C5A—C6A—C7A120.4 (4)
C5—C6—H6119.7C7A—C6A—H6A119.8
C5—C6—C7120.7 (3)C2A—C7A—H7A120.2
C7—C6—H6119.7C6A—C7A—C2A119.6 (4)
C2—C7—H7120.5C6A—C7A—H7A120.2
C6—C7—C2119.0 (3)N5A—C8A—N8A112.3 (3)
C6—C7—H7120.5N5A—C8A—C9A125.2 (3)
N5—C8—N8112.0 (3)N8A—C8A—C9A122.5 (3)
N5—C8—C9124.9 (3)C10A—C9A—C8A121.2 (3)
N8—C8—C9123.1 (3)C10A—C9A—C14A119.4 (3)
C10—C9—C8120.9 (3)C14A—C9A—C8A119.3 (3)
C10—C9—C14119.4 (3)C9A—C10A—H10A119.9
C14—C9—C8119.7 (3)C9A—C10A—C11A120.3 (4)
C9—C10—H10119.9C11A—C10A—H10A119.9
C11—C10—C9120.2 (4)C10A—C11A—H11A119.9
C11—C10—H10119.9C12A—C11A—C10A120.3 (4)
C10—C11—H11119.8C12A—C11A—H11A119.9
C12—C11—C10120.4 (4)C11A—C12A—H12A120.2
C12—C11—H11119.8C13A—C12A—C11A119.7 (4)
C11—C12—H12120.2C13A—C12A—H12A120.2
C11—C12—C13119.5 (3)C12A—C13A—H13A119.7
C13—C12—H12120.2C12A—C13A—C14A120.6 (4)
C12—C13—H13119.7C14A—C13A—H13A119.7
C12—C13—C14120.6 (4)C9A—C14A—H14A120.1
C14—C13—H13119.7C13A—C14A—C9A119.8 (4)
C9—C14—C13119.8 (4)C13A—C14A—H14A120.1
C9—C14—H14120.1N9A—C15A—N12A112.3 (3)
C13—C14—H14120.1N9A—C15A—C16A124.9 (3)
N9—C15—N12112.2 (3)N12A—C15A—C16A122.7 (3)
N9—C15—C16124.6 (3)C17A—C16A—C15A118.9 (3)
N12—C15—C16123.2 (3)C21A—C16A—C15A121.6 (3)
C17—C16—C15119.9 (3)C21A—C16A—C17A119.5 (3)
C21—C16—C15120.6 (3)C16A—C17A—H17A119.9
C21—C16—C17119.5 (3)C18A—C17A—C16A120.1 (4)
C16—C17—H17120.4C18A—C17A—H17A119.9
C18—C17—C16119.3 (4)C17A—C18A—H18A119.9
C18—C17—H17120.4C19A—C18A—C17A120.2 (4)
C17—C18—H18119.4C19A—C18A—H18A119.9
C17—C18—C19121.1 (4)C18A—C19A—H19A120.0
C19—C18—H18119.4C18A—C19A—C20A120.0 (4)
C18—C19—H19120.3C20A—C19A—H19A120.0
C20—C19—C18119.5 (4)C19A—C20A—H20A119.8
C20—C19—H19120.3C19A—C20A—C21A120.3 (4)
C19—C20—H20119.9C21A—C20A—H20A119.8
C19—C20—C21120.3 (4)C16A—C21A—C20A119.9 (4)
C21—C20—H20119.9C16A—C21A—H21A120.0
C16—C21—C20120.4 (4)C20A—C21A—H21A120.0
C16—C21—H21119.8N13A—C22A—H22D109.5
C20—C21—H21119.8N13A—C22A—H22E109.5
N13—C22—H22A109.5N13A—C22A—H22F109.5
N13—C22—H22B109.5H22D—C22A—H22E109.5
N13—C22—H22C109.5H22D—C22A—H22F109.5
H22A—C22—H22B109.5H22E—C22A—H22F109.5
H22A—C22—H22C109.5N13A—C23A—H23D109.5
H22B—C22—H22C109.5N13A—C23A—H23E109.5
N13—C23—H23A109.5N13A—C23A—H23F109.5
N13—C23—H23B109.5H23D—C23A—H23E109.5
N13—C23—H23C109.5H23D—C23A—H23F109.5
H23A—C23—H23B109.5H23E—C23A—H23F109.5
H23A—C23—H23C109.5N18A—C31A—N21A112.6 (3)
H23B—C23—H23C109.5N18A—C31A—C32A124.2 (3)
N14—C24—N17112.1 (3)N21A—C31A—C32A123.1 (3)
N14—C24—C25122.4 (3)C33A—C32A—C31A119.9 (3)
N17—C24—C25125.4 (3)C33A—C32A—C37A119.7 (3)
C26—C25—C24119.4 (3)C37A—C32A—C31A120.3 (3)
C26—C25—C30119.5 (3)C32A—C33A—H33A120.1
C30—C25—C24121.0 (3)C32A—C33A—C34A119.9 (3)
C25—C26—H26119.8C34A—C33A—H33A120.1
C27—C26—C25120.4 (3)C33A—C34A—H34A120.0
C27—C26—H26119.8C35A—C34A—C33A120.0 (3)
C26—C27—H27120.1C35A—C34A—H34A120.0
C26—C27—C28119.9 (3)C34A—C35A—H35A119.8
C28—C27—H27120.1C36A—C35A—C34A120.4 (3)
C27—C28—H28119.8C36A—C35A—H35A119.8
C29—C28—C27120.3 (3)C35A—C36A—H36A120.0
C29—C28—H28119.8C35A—C36A—C37A120.0 (4)
C28—C29—H29120.0C37A—C36A—H36A120.0
C28—C29—C30119.9 (4)C32A—C37A—H37A120.0
C30—C29—H29120.0C36A—C37A—C32A120.0 (4)
C25—C30—C29119.9 (3)C36A—C37A—H37A120.0
C25—C30—H30120.1N14A—C24A—N17A112.2 (3)
C29—C30—H30120.1N14A—C24A—C25A123.6 (3)
N18—C31—N21112.3 (3)N17A—C24A—C25A124.2 (3)
N18—C31—C32124.7 (3)C30A—C25A—C24A119.8 (3)
N21—C31—C32123.0 (3)C30A—C25A—C26A119.9 (3)
C33—C32—C31119.6 (3)C26A—C25A—C24A120.4 (3)
C33—C32—C37119.8 (3)C25A—C30A—H30A119.9
C37—C32—C31120.4 (3)C29A—C30A—C25A120.2 (4)
C32—C33—H33120.0C29A—C30A—H30A119.9
C32—C33—C34119.9 (4)C30A—C29A—H29A120.0
C34—C33—H33120.0C30A—C29A—C28A119.9 (4)
C33—C34—H34119.9C28A—C29A—H29A120.0
C35—C34—C33120.1 (4)C29A—C28A—H28A120.1
C35—C34—H34119.9C27A—C28A—C29A119.9 (3)
C34—C35—H35119.8C27A—C28A—H28A120.1
C34—C35—C36120.3 (4)C28A—C27A—H27A119.7
C36—C35—H35119.8C26A—C27A—C28A120.6 (3)
C35—C36—H36120.1C26A—C27A—H27A119.7
C35—C36—C37119.9 (4)C25A—C26A—H26A120.2
C37—C36—H36120.1C27A—C26A—C25A119.6 (3)
C32—C37—H37120.1C27A—C26A—H26A120.2
C36—C37—C32119.8 (4)N22A—C38A—N25A112.0 (3)
C36—C37—H37120.1N22A—C38A—C39A124.1 (3)
N22—C38—N25112.1 (3)N25A—C38A—C39A123.9 (3)
N22—C38—C39124.5 (3)C40A—C39A—C38A120.5 (3)
N25—C38—C39123.4 (3)C44A—C39A—C38A119.9 (3)
C40—C39—C38119.3 (3)C44A—C39A—C40A119.6 (3)
C44—C39—C38121.2 (3)C39A—C40A—H40A120.1
C44—C39—C40119.5 (3)C39A—C40A—C41A119.7 (4)
C39—C40—H40120.2C41A—C40A—H40A120.1
C41—C40—C39119.6 (3)C40A—C41A—H41A119.9
C41—C40—H40120.2C42A—C41A—C40A120.1 (4)
C40—C41—H41119.7C42A—C41A—H41A119.9
C42—C41—C40120.7 (3)C41A—C42A—H42A119.9
C42—C41—H41119.7C43A—C42A—C41A120.2 (4)
C41—C42—H42120.0C43A—C42A—H42A119.9
C41—C42—C43119.9 (3)C42A—C43A—H43A119.9
C43—C42—H42120.0C42A—C43A—C44A120.2 (4)
C42—C43—H43120.1C44A—C43A—H43A119.9
C44—C43—C42119.8 (3)C39A—C44A—H44A119.9
C44—C43—H43120.1C43A—C44A—C39A120.1 (4)
C39—C44—H44119.7C43A—C44A—H44A119.9
C43—C44—C39120.5 (3)N26A—C45A—N29A111.7 (3)
C43—C44—H44119.7N26A—C45A—C46A125.0 (3)
N26—C45—N29112.0 (3)N29A—C45A—C46A123.3 (3)
N26—C45—C46125.0 (3)C51A—C46A—C45A120.2 (3)
N29—C45—C46122.9 (3)C47A—C46A—C45A120.9 (3)
C47—C46—C45121.2 (3)C47A—C46A—C51A118.9 (3)
C47—C46—C51119.0 (3)C46A—C51A—H51A119.9
C51—C46—C45119.8 (3)C50A—C51A—C46A120.1 (3)
C46—C47—H47119.6C50A—C51A—H51A119.9
C46—C47—C48120.7 (4)C51A—C50A—H50A119.5
C48—C47—H47119.6C49A—C50A—C51A120.9 (4)
C47—C48—H48120.1C49A—C50A—H50A119.5
C49—C48—C47119.8 (4)C50A—C49A—H49A120.5
C49—C48—H48120.1C50A—C49A—C48A119.0 (4)
C48—C49—H49120.0C48A—C49A—H49A120.5
C48—C49—C50120.0 (4)C49A—C48A—H48A119.7
C50—C49—H49120.0C49A—C48A—C47A120.6 (4)
C49—C50—H50119.8C47A—C48A—H48A119.7
C49—C50—C51120.4 (4)C46A—C47A—H47A119.7
C51—C50—H50119.8C48A—C47A—C46A120.5 (3)
C46—C51—H51120.0C48A—C47A—H47A119.7
C50—C51—C46120.0 (3)N30A—C52A—N33A112.1 (3)
C50—C51—H51120.0N30A—C52A—C53A125.4 (3)
N30—C52—N33112.2 (3)N33A—C52A—C53A122.5 (3)
N30—C52—C53118.3 (4)C58A—C53A—C52A119.3 (3)
N30—C52—C53B129.6 (5)C54A—C53A—C52A121.3 (3)
N33—C52—C53129.4 (5)C54A—C53A—C58A119.5 (3)
N33—C52—C53B118.2 (5)C53A—C58A—H58A119.9
C54—C53—C52121.3 (5)C57A—C58A—C53A120.1 (4)
C54—C53—C58120.0C57A—C58A—H58A119.9
C58—C53—C52118.5 (5)C58A—C57A—H57A119.7
C53—C54—H54120.0C58A—C57A—C56A120.6 (4)
C53—C54—C55120.0C56A—C57A—H57A119.7
C55—C54—H54120.0C57A—C56A—H56A120.3
C54—C55—H55120.0C57A—C56A—C55A119.5 (3)
C56—C55—C54120.0C55A—C56A—H56A120.3
C56—C55—H55120.0C56A—C55A—H55A119.9
C55—C56—H56120.0C56A—C55A—C54A120.3 (4)
C55—C56—C57120.0C54A—C55A—H55A119.9
C57—C56—H56120.0C53A—C54A—C55A120.0 (4)
C56—C57—H57120.0C53A—C54A—H54A120.0
C58—C57—C56120.0C55A—C54A—H54A120.0
C58—C57—H57120.0N34A—C59A—H59D109.5
C53—C58—H58120.0N34A—C59A—H59E109.5
C57—C58—C53120.0N34A—C59A—H59F109.5
C57—C58—H58120.0H59D—C59A—H59E109.5
C54B—C53B—C52117.1 (5)H59D—C59A—H59F109.5
C54B—C53B—C58B120.0H59E—C59A—H59F109.5
C58B—C53B—C52122.8 (5)N34A—C60A—H60D109.5
C53B—C54B—H54B120.0N34A—C60A—H60E109.5
C53B—C54B—C55B120.0N34A—C60A—H60F109.5
C55B—C54B—H54B120.0H60D—C60A—H60E109.5
C54B—C55B—H55B120.0H60D—C60A—H60F109.5
C56B—C55B—C54B120.0H60E—C60A—H60F109.5
C56B—C55B—H55B120.0N35A—C61A—H61D109.5
C55B—C56B—H56B120.0N35A—C61A—H61E109.5
C55B—C56B—C57B120.0N35A—C61A—H61F109.5
C57B—C56B—H56B120.0H61D—C61A—H61E109.5
C56B—C57B—H57B120.0H61D—C61A—H61F109.5
C58B—C57B—C56B120.0H61E—C61A—H61F109.5
C58B—C57B—H57B120.0N35A—C62A—H62D109.5
C53B—C58B—H58B120.0N35A—C62A—H62E109.5
C57B—C58B—C53B120.0N35A—C62A—H62F109.5
C57B—C58B—H58B120.0H62D—C62A—H62E109.5
N34—C59—H59A109.5H62D—C62A—H62F109.5
N34—C59—H59B109.5H62E—C62A—H62F109.5
N34—C59—H59C109.5N36A—C63A—H63D109.5
H59A—C59—H59B109.5N36A—C63A—H63E109.5
H59A—C59—H59C109.5N36A—C63A—H63F109.5
H59B—C59—H59C109.5H63D—C63A—H63E109.5
N34—C60—H60A109.5H63D—C63A—H63F109.5
N34—C60—H60B109.5H63E—C63A—H63F109.5
N34—C60—H60C109.5N36A—C64A—H64D109.5
H60A—C60—H60B109.5N36A—C64A—H64E109.5
H60A—C60—H60C109.5N36A—C64A—H64F109.5
H60B—C60—H60C109.5H64D—C64A—H64E109.5
N35—C61—H61A109.5H64D—C64A—H64F109.5
N35—C61—H61B109.5H64E—C64A—H64F109.5
N35—C61—H61C109.5H1SA—C1S—H1SB109.5
H61A—C61—H61B109.5H1SA—C1S—H1SC109.5
H61A—C61—H61C109.5H1SB—C1S—H1SC109.5
H61B—C61—H61C109.5C2S—C1S—H1SA109.5
N35—C62—H62A109.5C2S—C1S—H1SB109.5
N35—C62—H62B109.5C2S—C1S—H1SC109.5
N35—C62—H62C109.5C3S—C2S—C1S121.0
H62A—C62—H62B109.5C7S—C2S—C1S120.9
H62A—C62—H62C109.5C7S—C2S—C3S118.1
H62B—C62—H62C109.5C2S—C3S—H3S119.5
N36—C63—H63A109.5C4S—C3S—C2S121.1
N36—C63—H63B109.5C4S—C3S—H3S119.5
N36—C63—H63C109.5C3S—C4S—H4S119.9
H63A—C63—H63B109.5C5S—C4S—C3S120.1
H63A—C63—H63C109.5C5S—C4S—H4S119.9
H63B—C63—H63C109.5C4S—C5S—H5S120.3
N36—C64—H64A109.5C4S—C5S—C6S119.4
N36—C64—H64B109.5C6S—C5S—H5S120.3
N36—C64—H64C109.5C5S—C6S—H6S119.9
H64A—C64—H64B109.5C7S—C6S—C5S120.1
H64A—C64—H64C109.5C7S—C6S—H6S119.9
H64B—C64—H64C109.5C2S—C7S—H7S119.5
O1A—Ta1A—N2A101.40 (9)C6S—C7S—C2S121.1
O1A—Ta1A—N6A87.99 (10)C6S—C7S—H7S119.5
Ta1—N2—N3—N4167.1 (2)C55B—C56B—C57B—C58B0.0
Ta1—N6—N7—N8176.3 (2)C56B—C57B—C58B—C53B0.0
Ta1—N10—N11—N12178.9 (2)C58B—C53B—C54B—C55B0.0
Ta1—N15—N16—Ta24.2 (3)Ta1A—N2A—N3A—N4A178.2 (2)
Ta1—N15—N16—N17171.25 (19)Ta1A—N6A—N7A—N8A175.3 (2)
Ta1—N19—N20—Ta22.9 (3)Ta1A—N10A—N11A—N12A172.6 (2)
Ta1—N19—N20—N21179.4 (2)Ta1A—N19A—N20A—Ta2A3.9 (3)
Ta2—N16—N17—C24174.9 (2)Ta1A—N19A—N20A—N21A177.70 (19)
Ta2—N20—N21—C31176.9 (2)Ta1A—N15A—N16A—Ta2A1.0 (3)
Ta2—N23—N24—N25167.2 (2)Ta1A—N15A—N16A—N17A169.22 (19)
Ta2—N27—N28—N29164.6 (2)Ta2A—N20A—N21A—C31A178.1 (2)
Ta2—N31—N32—N33173.9 (2)Ta2A—N16A—N17A—C24A169.0 (2)
N1—N2—N3—N40.2 (4)Ta2A—N23A—N24A—N25A170.1 (2)
N1—C1—C2—C319.1 (5)Ta2A—N27A—N28A—N29A178.3 (2)
N1—C1—C2—C7164.9 (3)Ta2A—N31A—N32A—N33A177.6 (2)
N2—N1—C1—N40.1 (4)N1A—N2A—N3A—N4A1.5 (4)
N2—N1—C1—C2175.1 (3)N1A—C1A—C2A—C3A18.4 (5)
N2—N3—N4—C10.1 (4)N1A—C1A—C2A—C7A164.0 (3)
N3—N4—C1—N10.0 (4)N2A—N1A—C1A—N4A1.1 (4)
N3—N4—C1—C2174.9 (3)N2A—N1A—C1A—C2A177.7 (3)
N4—C1—C2—C3155.3 (3)N2A—N3A—N4A—C1A0.8 (4)
N4—C1—C2—C720.7 (5)N3A—N4A—C1A—N1A0.2 (4)
N5—N6—N7—N80.2 (4)N3A—N4A—C1A—C2A176.9 (3)
N5—C8—C9—C107.0 (5)N4A—C1A—C2A—C3A157.9 (4)
N5—C8—C9—C14171.7 (3)N4A—C1A—C2A—C7A19.6 (5)
N6—N5—C8—N80.1 (4)N5A—N6A—N7A—N8A1.5 (4)
N6—N5—C8—C9177.7 (3)N5A—C8A—C9A—C10A12.4 (5)
N6—N7—N8—C80.1 (4)N5A—C8A—C9A—C14A167.2 (4)
N7—N8—C8—N50.0 (4)N6A—N5A—C8A—N8A2.1 (4)
N7—N8—C8—C9177.8 (3)N6A—N5A—C8A—C9A178.9 (3)
N8—C8—C9—C10175.4 (3)N6A—N7A—N8A—C8A0.1 (4)
N8—C8—C9—C145.9 (5)N7A—N8A—C8A—N5A1.3 (4)
N9—N10—N11—N120.1 (4)N7A—N8A—C8A—C9A179.7 (3)
N9—C15—C16—C17168.1 (3)N8A—C8A—C9A—C10A166.4 (3)
N9—C15—C16—C2113.3 (5)N8A—C8A—C9A—C14A14.0 (5)
N10—N9—C15—N120.4 (4)N9A—N10A—N11A—N12A0.4 (4)
N10—N9—C15—C16179.4 (3)N9A—C15A—C16A—C17A158.5 (3)
N10—N11—N12—C150.1 (4)N9A—C15A—C16A—C21A21.8 (5)
N11—N12—C15—N90.3 (4)N10A—N9A—C15A—N12A0.2 (4)
N11—N12—C15—C16179.3 (3)N10A—N9A—C15A—C16A178.8 (3)
N12—C15—C16—C1713.0 (5)N10A—N11A—N12A—C15A0.5 (4)
N12—C15—C16—C21165.6 (4)N11A—N12A—C15A—N9A0.4 (4)
N14—N15—N16—Ta2175.65 (19)N11A—N12A—C15A—C16A178.6 (3)
N14—N15—N16—N170.2 (3)N12A—C15A—C16A—C17A20.4 (5)
N14—C24—C25—C265.7 (5)N12A—C15A—C16A—C21A159.3 (3)
N14—C24—C25—C30173.0 (3)N18A—N19A—N20A—Ta2A177.79 (19)
N15—N14—C24—N170.2 (4)N18A—N19A—N20A—N21A0.6 (3)
N15—N14—C24—C25177.5 (3)N18A—C31A—C32A—C33A8.4 (5)
N15—N16—N17—C240.1 (3)N18A—C31A—C32A—C37A175.1 (3)
N16—N17—C24—N140.0 (4)N19A—N18A—C31A—N21A0.8 (4)
N16—N17—C24—C25177.5 (3)N19A—N18A—C31A—C32A178.7 (3)
N17—C24—C25—C26171.6 (3)N19A—N20A—N21A—C31A0.1 (3)
N17—C24—C25—C309.7 (5)N20A—N21A—C31A—N18A0.4 (4)
N18—N19—N20—Ta2176.91 (19)N20A—N21A—C31A—C32A178.4 (3)
N18—N19—N20—N210.8 (4)N21A—C31A—C32A—C33A169.3 (3)
N18—C31—C32—C3321.4 (5)N21A—C31A—C32A—C37A7.2 (5)
N18—C31—C32—C37162.3 (4)N14A—N15A—N16A—Ta2A170.18 (19)
N19—N18—C31—N210.3 (4)N14A—N15A—N16A—N17A0.1 (3)
N19—N18—C31—C32178.4 (3)N14A—C24A—C25A—C30A159.8 (3)
N19—N20—N21—C310.6 (3)N14A—C24A—C25A—C26A19.4 (5)
N20—N21—C31—N180.2 (4)N15A—N14A—C24A—N17A0.1 (4)
N20—N21—C31—C32178.9 (3)N15A—N14A—C24A—C25A178.0 (3)
N21—C31—C32—C33157.2 (3)N15A—N16A—N17A—C24A0.1 (3)
N21—C31—C32—C3719.1 (5)N16A—N17A—C24A—N14A0.2 (4)
N22—N23—N24—N250.0 (4)N16A—N17A—C24A—C25A177.9 (3)
N22—C38—C39—C40175.1 (3)N17A—C24A—C25A—C30A18.1 (5)
N22—C38—C39—C444.9 (5)N17A—C24A—C25A—C26A162.7 (3)
N23—N22—C38—N250.6 (4)N22A—N23A—N24A—N25A0.7 (4)
N23—N22—C38—C39178.4 (3)N22A—C38A—C39A—C40A162.9 (3)
N23—N24—N25—C380.4 (4)N22A—C38A—C39A—C44A16.3 (5)
N24—N25—C38—N220.6 (4)N23A—N22A—C38A—N25A0.7 (4)
N24—N25—C38—C39178.4 (3)N23A—N22A—C38A—C39A179.5 (3)
N25—C38—C39—C403.8 (5)N23A—N24A—N25A—C38A0.2 (4)
N25—C38—C39—C44176.3 (3)N24A—N25A—C38A—N22A0.3 (4)
N26—N27—N28—N290.9 (4)N24A—N25A—C38A—C39A179.9 (3)
N26—C45—C46—C4715.9 (5)N25A—C38A—C39A—C40A17.3 (5)
N26—C45—C46—C51162.9 (3)N25A—C38A—C39A—C44A163.5 (4)
N27—N26—C45—N290.7 (4)N26A—N27A—N28A—N29A0.9 (4)
N27—N26—C45—C46178.9 (3)N26A—C45A—C46A—C51A179.1 (3)
N27—N28—N29—C450.5 (4)N26A—C45A—C46A—C47A2.6 (5)
N28—N29—C45—N260.1 (4)N27A—N26A—C45A—N29A1.2 (4)
N28—N29—C45—C46178.4 (3)N27A—N26A—C45A—C46A179.0 (3)
N29—C45—C46—C47166.0 (4)N27A—N28A—N29A—C45A0.2 (4)
N29—C45—C46—C5115.2 (5)N28A—N29A—C45A—N26A0.7 (4)
N30—N31—N32—N330.3 (4)N28A—N29A—C45A—C46A179.6 (3)
N30—C52—C53—C546.9 (7)N29A—C45A—C46A—C51A0.7 (5)
N30—C52—C53—C58177.3 (4)N29A—C45A—C46A—C47A177.6 (3)
N30—C52—C53B—C54B2.8 (8)N30A—N31A—N32A—N33A0.0 (4)
N30—C52—C53B—C58B173.6 (4)N30A—C52A—C53A—C58A178.2 (3)
N31—N30—C52—N330.7 (4)N30A—C52A—C53A—C54A1.5 (5)
N31—N30—C52—C53177.2 (4)N31A—N30A—C52A—N33A0.1 (4)
N31—N30—C52—C53B177.8 (5)N31A—N30A—C52A—C53A179.3 (3)
N31—N32—N33—C520.2 (4)N31A—N32A—N33A—C52A0.0 (4)
N32—N33—C52—N300.6 (4)N32A—N33A—C52A—N30A0.1 (4)
N32—N33—C52—C53176.5 (5)N32A—N33A—C52A—C53A179.3 (3)
N32—N33—C52—C53B178.0 (5)N33A—C52A—C53A—C58A1.1 (5)
N33—C52—C53—C54168.8 (5)N33A—C52A—C53A—C54A179.2 (3)
N33—C52—C53—C587.0 (8)C1A—N1A—N2A—Ta1A178.2 (2)
N33—C52—C53B—C54B179.8 (4)C1A—N1A—N2A—N3A1.5 (4)
N33—C52—C53B—C58B3.4 (7)C1A—C2A—C3A—C4A177.6 (3)
C1—N1—N2—Ta1167.0 (2)C1A—C2A—C7A—C6A177.7 (3)
C1—N1—N2—N30.1 (4)C2A—C3A—C4A—C5A0.3 (5)
C1—C2—C3—C4175.0 (3)C3A—C2A—C7A—C6A0.1 (5)
C1—C2—C7—C6175.2 (3)C3A—C4A—C5A—C6A0.5 (6)
C2—C3—C4—C50.0 (5)C4A—C5A—C6A—C7A0.4 (6)
C3—C2—C7—C60.8 (5)C5A—C6A—C7A—C2A0.1 (6)
C3—C4—C5—C61.0 (6)C7A—C2A—C3A—C4A0.0 (5)
C4—C5—C6—C71.1 (6)C8A—N5A—N6A—Ta1A174.4 (2)
C5—C6—C7—C20.2 (5)C8A—N5A—N6A—N7A2.2 (4)
C7—C2—C3—C41.0 (5)C8A—C9A—C10A—C11A179.0 (3)
C8—N5—N6—Ta1176.3 (2)C8A—C9A—C14A—C13A178.7 (4)
C8—N5—N6—N70.2 (3)C9A—C10A—C11A—C12A0.6 (5)
C8—C9—C10—C11178.4 (3)C10A—C9A—C14A—C13A0.9 (6)
C8—C9—C14—C13178.3 (3)C10A—C11A—C12A—C13A1.5 (6)
C9—C10—C11—C120.0 (6)C11A—C12A—C13A—C14A1.2 (7)
C10—C9—C14—C130.4 (6)C12A—C13A—C14A—C9A0.0 (7)
C10—C11—C12—C130.4 (6)C14A—C9A—C10A—C11A0.6 (5)
C11—C12—C13—C140.3 (6)C15A—N9A—N10A—Ta1A172.6 (2)
C12—C13—C14—C90.1 (6)C15A—N9A—N10A—N11A0.1 (3)
C14—C9—C10—C110.4 (5)C15A—C16A—C17A—C18A179.7 (3)
C15—N9—N10—Ta1179.0 (2)C15A—C16A—C21A—C20A179.5 (4)
C15—N9—N10—N110.3 (3)C16A—C17A—C18A—C19A0.0 (6)
C15—C16—C17—C18179.1 (3)C17A—C16A—C21A—C20A0.9 (6)
C15—C16—C21—C20179.9 (4)C17A—C18A—C19A—C20A0.4 (6)
C16—C17—C18—C190.6 (6)C18A—C19A—C20A—C21A0.1 (7)
C17—C16—C21—C201.4 (6)C19A—C20A—C21A—C16A0.5 (6)
C17—C18—C19—C200.7 (7)C21A—C16A—C17A—C18A0.6 (6)
C18—C19—C20—C210.1 (7)C31A—N18A—N19A—Ta1A177.3 (2)
C19—C20—C21—C161.2 (7)C31A—N18A—N19A—N20A0.8 (3)
C21—C16—C17—C180.5 (6)C31A—C32A—C33A—C34A175.8 (3)
C24—N14—N15—Ta1170.5 (2)C31A—C32A—C37A—C36A176.4 (4)
C24—N14—N15—N160.2 (3)C32A—C33A—C34A—C35A0.2 (5)
C24—C25—C26—C27179.6 (3)C33A—C32A—C37A—C36A0.1 (6)
C24—C25—C30—C29179.9 (3)C33A—C34A—C35A—C36A1.1 (6)
C25—C26—C27—C280.2 (5)C34A—C35A—C36A—C37A1.8 (6)
C26—C25—C30—C291.2 (5)C35A—C36A—C37A—C32A1.2 (6)
C26—C27—C28—C290.9 (6)C37A—C32A—C33A—C34A0.8 (5)
C27—C28—C29—C300.5 (6)C24A—N14A—N15A—Ta1A168.2 (2)
C28—C29—C30—C250.5 (6)C24A—N14A—N15A—N16A0.0 (3)
C30—C25—C26—C270.9 (5)C24A—C25A—C30A—C29A179.5 (4)
C31—N18—N19—Ta1179.6 (2)C24A—C25A—C26A—C27A178.7 (3)
C31—N18—N19—N200.7 (3)C25A—C30A—C29A—C28A0.8 (7)
C31—C32—C33—C34174.7 (3)C30A—C25A—C26A—C27A2.0 (5)
C31—C32—C37—C36176.0 (4)C30A—C29A—C28A—C27A2.0 (7)
C32—C33—C34—C351.0 (6)C29A—C28A—C27A—C26A1.2 (6)
C33—C32—C37—C360.3 (6)C28A—C27A—C26A—C25A0.8 (5)
C33—C34—C35—C360.8 (6)C26A—C25A—C30A—C29A1.2 (6)
C34—C35—C36—C372.2 (7)C38A—N22A—N23A—Ta2A170.3 (2)
C35—C36—C37—C321.6 (7)C38A—N22A—N23A—N24A0.9 (4)
C37—C32—C33—C341.6 (5)C38A—C39A—C40A—C41A179.6 (4)
C38—N22—N23—Ta2167.2 (2)C38A—C39A—C44A—C43A179.9 (3)
C38—N22—N23—N240.3 (4)C39A—C40A—C41A—C42A0.1 (7)
C38—C39—C40—C41178.3 (3)C40A—C39A—C44A—C43A0.7 (6)
C38—C39—C44—C43179.9 (3)C40A—C41A—C42A—C43A0.0 (7)
C39—C40—C41—C421.5 (6)C41A—C42A—C43A—C44A0.3 (7)
C40—C39—C44—C430.2 (5)C42A—C43A—C44A—C39A0.6 (6)
C40—C41—C42—C430.1 (6)C44A—C39A—C40A—C41A0.4 (6)
C41—C42—C43—C441.6 (6)C45A—N26A—N27A—Ta2A177.9 (2)
C42—C43—C44—C391.5 (6)C45A—N26A—N27A—N28A1.3 (3)
C44—C39—C40—C411.7 (5)C45A—C46A—C51A—C50A178.9 (3)
C45—N26—N27—Ta2164.3 (2)C45A—C46A—C47A—C48A178.5 (3)
C45—N26—N27—N281.0 (4)C46A—C51A—C50A—C49A0.7 (6)
C45—C46—C47—C48179.3 (4)C51A—C46A—C47A—C48A0.1 (5)
C45—C46—C51—C50179.8 (3)C51A—C50A—C49A—C48A0.4 (7)
C46—C47—C48—C491.6 (7)C50A—C49A—C48A—C47A0.0 (6)
C47—C46—C51—C501.0 (5)C49A—C48A—C47A—C46A0.1 (6)
C47—C48—C49—C500.3 (7)C47A—C46A—C51A—C50A0.5 (5)
C48—C49—C50—C510.7 (7)C52A—N30A—N31A—Ta2A177.4 (2)
C49—C50—C51—C460.3 (6)C52A—N30A—N31A—N32A0.1 (3)
C51—C46—C47—C481.9 (6)C52A—C53A—C58A—C57A179.5 (3)
C52—N30—N31—Ta2174.1 (2)C52A—C53A—C54A—C55A179.9 (3)
C52—N30—N31—N320.6 (4)C53A—C58A—C57A—C56A0.1 (6)
C52—C53—C54—C55175.7 (7)C58A—C53A—C54A—C55A0.1 (5)
C52—C53—C58—C57175.8 (7)C58A—C57A—C56A—C55A0.5 (6)
C52—C53B—C54B—C55B176.5 (7)C57A—C56A—C55A—C54A1.0 (6)
C52—C53B—C58B—C57B176.3 (7)C56A—C55A—C54A—C53A0.8 (5)
C53—C54—C55—C560.0C54A—C53A—C58A—C57A0.3 (5)
C54—C53—C58—C570.0C1S—C2S—C3S—C4S178.6
C54—C55—C56—C570.0C1S—C2S—C7S—C6S178.6
C55—C56—C57—C580.0C2S—C3S—C4S—C5S0.1
C56—C57—C58—C530.0C3S—C2S—C7S—C6S0.2
C58—C53—C54—C550.0C3S—C4S—C5S—C6S0.1
C53B—C54B—C55B—C56B0.0C4S—C5S—C6S—C7S0.1
C54B—C53B—C58B—C57B0.0C5S—C6S—C7S—C2S0.0
C54B—C55B—C56B—C57B0.0C7S—C2S—C3S—C4S0.2
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N35—H35B···N240.912.002.875 (4)161
N35—H35C···N30.912.463.031 (4)121
N35—H35C···N70.912.122.943 (4)150
N36—H36B···N110.911.982.836 (4)156
N36—H36C···N280.912.172.978 (5)148
N36—H36C···N320.912.443.085 (4)128
N35A—H35D···N3A0.912.052.867 (4)149
N35A—H35E···N24A0.912.332.994 (4)130
N35A—H35E···N28A0.912.202.954 (4)140
N36A—H36D···N7A0.912.232.961 (4)137
N36A—H36D···N11A0.912.342.981 (4)127
N36A—H36E···N32A0.911.952.828 (4)161
Ligand composition of complexes 13 top
Compound
123
Charges-100-2
LigandsMetal center
TiZr1Zr2Ta
NMe22111
HNMe20110
µ-Tz3332
η1-Tz terminal1203
η2-Tz terminal0010
µ-oxo0001
Number of hydrogen-bonded Me2NH2+1002
 

Acknowledgements

The Bruker Quazar APEX2 was purchased by the UW–Madison Department of Chemistry with a portion of a generous gift from Paul J. and Margaret M. Bender. We thank Professor Clark Landis (University of Wisconsin–Madison) and Professor Charles H. Winter (Wayne State University) for fruitful discussions.

References

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