research communications
[Li6(C2N2H8)11.5][Fe4Se8]: the first lithium-containing chalcogenidotetraferrate synthesized in solution
aFabeckstr. 34-36, 14195 Berlin, Germany
*Correspondence e-mail: guenther.thiele@fu-berlin.de
The octaselenidotetraferrate(II/III) with six Li atoms as counter-ions chelated by ethylenediamine (en, C2H8N2), {[Li6(en)11.5][Fe4Se8]}n, was synthesized from Li, FeSe and Se in an ethylenediamine solution at room temperature. Its was determined at 100 K and has triclinic (P) symmetry. The [Fe4Se8]6− anions show a connectivity comparable to a distorted tetrahedral cluster structure. Contact distances are given, and central structure features compared to literature known selenidoferrates with the same anion motif.
Keywords: crystal structure; selenido ferrates; heterocubane clusters.
CCDC reference: 2217266
1. Chemical context
Alkali metal chalcogenido ferrates Ax[FeyChz] (A = Li⋯Cs; Ch = O⋯Te) show [FeCh4] tetrahedra to be the most prominent coordination motif of the anionic moiety. These can be isolated, connected into chains, layers, or three-dimensional networks. A special motive is the connection of four such [FeCh4] (Ch = S, Se, Te) units via three shared edges each to form a tetramer. This secondary structure can be described as a distorted heterocubane [Fe4Ch4]x− core, with one additional chalcogenido ligand on every iron corner of the heterocubane (Schwarz & Röhr, 2015). Another approach to describe those tetramers can be as a distorted tetrahedral star (stella quadrangula; Stüble et al., 2016).
The first reported ferrate of this type was Cs7[Fe4Te8] published by Bronger et al. in 1983. A7[Fe4Ch8] (A = K, Rb, Cs; Ch = S, Se, Te) is the most common sum formula for those ferrates. The respective sulfido and selenido ferrates are only known with Cs as alkali metal [Cs7[Fe4S8] (Schwarz & Röhr, 2015), Cs7[Fe4Se8] (Stüble & Röhr, 2017)], while the tellurido ferrates are known with K, Rb and Cs as alkali metals [K7[Fe4Te8], Rb7[Fe4Te8] (Stüble et al., 2016), Cs7[Fe4Te8] (Bronger et al., 1983)]. The reported tetrachalcogenido ferrates are synthesized in solid-state reactions at temperatures in the range 500–1050 K. With the exception of the potassium tellurido tetraferrates, all these alkali metal chalcogenido tetraferrates crystallize in the space-group type C2/c (Schwarz & Röhr, 2015; Stüble & Röhr, 2017; Stüble et al., 2016, 2018; Bronger et al., 1983). For K7[Fe4Te8], a room-temperature (P42/nmc) and a low-temperature (100 K, Pbcn) polymorph are known. K6[Fe4Se8] (Pbcn) is almost isostructural to the low-temperature modification of K7[Fe4Se8] with a missing K site (Stüble et al., 2016).
For the compound presented herein, an initial attempt was to use the solubility of Li and Se in ethylenediamine to form in situ Li2Se, which would then react with iron(II) selenide to a lithium selenidoferrate(II). Instead, the solution approach yielded the mixed-valent tetraferrate [Li6(en11.5)][Fe4Se8].
2. Structural commentary
The title compound (Fig. 1) crystallizes in the triclinic P. The consists of the cationic [Li6(en)11.5]6+ moiety forming networks and the anionic [Fe4Se8]6− unit, where each Fe atom is coordinated by four Se atoms, forming a distorted tetrahedron. The distortion is towards a trigonal–pyramidal geometry. The distorted [FeSe4] tetrahedra are connected via three edges with neighbouring tetrahedra, forming a distorted tetrahedral star [Fe4Se8]6– (stella quadrangula; Stüble et al., 2016) as a secondary structure (Fig. 2). The terminal Fe—Se distances are 2.3251 (8)–2.3502 (7) Å. The terminal Se3 directly coordinates Li3, at a distance of 2.634 (7) Å, positioned between two anions along the crystallographic b-axis (see Fig. 4). The Fe—Se bond lengths within the heterocubane core are in the range 2.3899 (8)—2.4752 (8) Å. Parallel to the b-axis the Fe—Se bonds are slightly shorter [2.3899 (8)—2.4157 (8) Å] than the rest of the bonds in the heterocubane [2.4414 (7)—2.4752 (8) Å] (see Figs. 3 and 4), this might be due to partial electron-density polarization towards the Li atom directly coordinated by one terminal Se ligand.
The Se—Fe—Se angles for the bridging Se atoms are in the range of 101.23 (2)—108.66 (3)° and therefore smaller than the ideal tetrahedron angle. As a result of the contraction of the heterocubane along the crystallographic b-axis, the Se—Fe—Se angles are the smallest in this direction, 101.23 (2)–101.90 (2)°. The Se—Fe—Se angles of the terminal Se atoms are in the range of 108.31 (2)—119.59 (3)°.
Five of the six crystallographically independent Li cations are tetrahedrally coordinated by one amine group of four ethylenediamine molecules. The ethylenediamine molecules bridge adjacent lithium cations to form an infinite three-dimensionally connected network of 3∞[Li6(en)11.5]6+. The last Li cation is coordinated by three amine groups of three independent ethylenediamine molecules with the fourth coordination site occupied by one of the terminal selenido ligands (Se3) as depicted in Fig. 4. The coordination of Se to the Li cation results in the non-integer number of ethylenediamine ligands in the sum formula. As a result of the individual coordination environments of lithium ions, a complicated 6-nodal net with point symbol {3.6.73.8}2{3.73.82}{42.6.82.9}{42.63.8}{6.8.9} is obtained (ToposPro V 5.4.1.0; Blatov et al., 2014).
3. Supramolecular features
The anion packing can be described as layers stacked in an AB type. The Li coordinated to the terminal Se ligand pointing in one direction defines the A layer, while the ligand pointing in the opposite direction defines the B layer. The layers are shifted with respect to each other such that the anions of one layer are placed between the anions of the other layer. The formation of those layers correlates with the inversion centre in the containing two asymmetric units. The Li–ethylenediamine network is located both in between and within those layers surrounding the anions (see Fig. 5). It is stabilized by classical N—H⋯Se and non-classical C—H⋯Se hydrogen bonds (Table 1).
The hydrogen bonds between the ethylenediamine molecules of the cationic network and the selenium atoms of the anion can be described by graph-set theory (e.g. Etter et al., 1990). In graph-set theory, a hydrogen-bond network can be described by a pattern designator (G), the pattern's degree (r) and the number of donors (d) and acceptors (a): Gad(r). G can be S (intramolecular), C (chains), R (rings) or D (non-cyclic) and r is the number of atoms before repetition. To be able to determine the graph sets, the Li—N coordination was also counted as a `bond' in the network, so rings or chains can contain Li atoms. The anionic moiety was not counted as taking part in the network; every acceptor Se atom was looked at individually. Only the smallest/simplest pattern for each set is given. For Se1 the graph set is three times R21(8), for the donor pairs N7, N14; N14, N16; N7, N16. Se2 can be described by two sets of R21(4) for N10, N18; N22, N23 and two R21(5) for N7, N13 and N21, N23. Se3 is bound in two sets of R21(4) to N2, N8; N15, N17 and in R21(5) to N2, N15 and R21(9) to N2, N24. Se4 has two sets, R21(8) N2, N8 and R21(12) N2, N6/N6A (the split positions of N6 are counted in a single set). Se5 has five sets of classical hydrogen bonds: three sets of R21(4) for N1, N19; N3, N19 and N12, N13; two sets of R21(5) for N2, N22 and N16, N19 and one set of non-classical hydrogen bonds D for C6. Se6 has one set of classical hydrogen bonds, R21(5) to N1, N18 and one set of non-classical D to C20. Se7 has one set of R21(5) for N4, N17 and one R21(7) for N12, N24A and one R21(9) N12, N20. Se8 has three classical sets of hydrogen bonds: one set of R21(4) to N4, N21, C22(4) for N5, N9 and R21(5) to N10, N14 and two non-classical sets, C22(8) to C1, C10/C10A (the split positions of C10 are counted in a single set) and C22(10) C1, C13.
4. Database survey
A search of the Cambridge Structural Database (CSD version 5.43; Groom et al., 2016) for compounds showing the motif of a heterocubane core containing iron and chalcogens yielded 548 results. Most of those are structures containing sulfidoferrate heterocubane cores, which are investigated with regard to iron–sulfur proteins. For a more direct comparison, only compounds comprising one terminal ligand on each iron atom and solely Se as the chalcogen were chosen, as the bond lengths inside the cubane core differ significantly depending on whether S or Se is part of the heterocubane. First, selenido ferrates, which only differ in the anionic moiety, are compared. In the second step, we analyse compounds that contain organic ligands on the terminal Se atoms.
Regarding the elemental ratios of alkali metal to Fe and Se, [Li6(en11.5)][Fe4Se8] is identical to K6[Fe4Se8] (ICSD: 430631; Stüble et al., 2016). In the following, the bond lengths of the anion are compared to the ones in K6[Fe4Se8], despite the differences in the cationic moiety. The Fe—Se bonds to the terminal Se atoms in the potassium selenido tetraferrate are in the range of 2.320 (2)–2.307 (2) Å and therefore shorter than the respective bonds in the title compound, lithium selenido tetraferrate [2.3251 (8)–2.3502 (7) Å]. The Fe—Se distances of the bridging Se atoms are in the range of 2.397 (2)–2.468 (2) Å in the potassium ferrate and 2.3899 (8)–2.4752 (8) Å in the lithium selenido tetraferrate. In known literature for the A7[Fe4Ch8] species, the anion is surrounded by 26 cations, which form a cube with one cation on each corner, edge, and face of the cube: Cs7[Fe4S8] (ICSD: 428508; Schwarz & Röhr, 2015), Cs7[Fe4Se8] (ICSD: 433140; Stüble & Röhr, 2017), (K7[Fe4Te8] (ICSD: 430632), Rb7[Fe4Te8] (ICSD: 430634; Stüble et al., 2016), Cs7[Fe4Te8] (ICSD: 37065; Bronger et al., 1983). In K6[Fe4Se8], 24 cations form a distorted cube around the anions. In the title compound, no such regular shape can be observed for the surrounding cations, probably due to the more complex cation motif with the ethylenediamine ligands interlinking the alkali metal ions.
Comparing the bond angles and distances of the anionic moiety to homologues with aliphatic or arylic ligands at the terminal Se atoms, the bond lengths inside the heterocubane core are in a similar range: Fe—Se distances are found to be 2.3573 (12)–2.4391 (12) Å in [Yb(THF)6][Fe4Se4(SePh4)4] (THF = tetrahydrofuran; CCDC 228675; Kornienko et al., 2003) and 2.391–2.434 Å in (NBu4)2[Fe4Se4(SeCH3)4] (CCDC 201198; Kern et al., 2004). In contrast, terminal Fe—Se distances are significantly elongated upon organic substitution: 2.3843 (12)–2.4055 (12) Å for [Yb(THF)6][Fe4Se4(SePh4)4] and 2.375 Å in (NBu4)2[Fe4Se4(SeCH3)4].
5. Synthesis and crystallization
500 mg (3.71 mmol, 1 eq.) of iron(II) selenide, 293 mg (3.71 mmol, 1 eq.) of Se and 52 mg (7.49 mmol, 2 eq.) of Li were stirred in 50 mL of dry ethylenediamine under an argon atmosphere. The reaction mixture was stirred for 24 h, during which time several colour changes from brown to green to brown occur; these are most likely associated with the various intermediate polyselenide anions. After 24 h, a final colour change to brown was observed and the solution was filtered and allowed to stand for 16 weeks to afford crystallization. A crystal suitable for X-ray
was chosen in Paratone oil under a light microscope. The obtained crystals were comparably large and visible without a microscope. Breaking the crystal typically yielded very small crystallites that immediately decomposed because of their air and moisture sensitivity. Therefore, a crystal larger than the X-ray beam was used for analysis.6. Refinement
Crystal data, data collection and structure .
details are summarized in Table 2
|
The crystal was found to comprise two pieces, mis-aligned by ∼1.6°. For the purpose of integration, and processing, facilities for handling SHELXL) were attempted. In combination with the experimentation with different integration box sizes with common-volume overlap of 4% did not result in an improved dataset.
by non-merohedry (namely the HKLF 5 data format inOne of the en ligands is disordered, the disorder was treated with RIGU and DELU restraints. H atoms were treated by a mixture of independent and constrained refinement.
Supporting information
CCDC reference: 2217266
https://doi.org/10.1107/S205698902201060X/jq2021sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S205698902201060X/jq2021Isup2.hkl
Data collection: APEX4 (Bruker, 2021); cell
SAINT (Bruker, 2016); data reduction: SAINT (Bruker, 2016); program(s) used to solve structure: SHELXT2018/2 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: Olex2 (Dolomanov et al., 2009); software used to prepare material for publication: Olex2 (Dolomanov et al., 2009).[Li6(C2H8N2)11.5][Fe4Se8] | Z = 2 |
Mr = 1587.91 | F(000) = 1570 |
Triclinic, P1 | Dx = 1.824 Mg m−3 |
a = 11.495 (2) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.665 (3) Å | Cell parameters from 9368 reflections |
c = 22.233 (5) Å | θ = 2.4–25.4° |
α = 92.885 (8)° | µ = 6.06 mm−1 |
β = 92.383 (7)° | T = 100 K |
γ = 103.510 (7)° | Block, dark black |
V = 2890.9 (11) Å3 | 0.8 × 0.6 × 0.4 mm |
Bruker APEXII CCD diffractometer | 9144 reflections with I > 2σ(I) |
Radiation source: sealed X-ray tube | Rint = 0.081 |
φ and ω scans | θmax = 25.5°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −13→13 |
Tmin = 0.323, Tmax = 0.745 | k = −14→14 |
178309 measured reflections | l = −26→26 |
10708 independent reflections |
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.030 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.059 | w = 1/[σ2(Fo2) + 11.5642P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max = 0.002 |
10708 reflections | Δρmax = 0.65 e Å−3 |
752 parameters | Δρmin = −0.64 e Å−3 |
193 restraints |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Se1 | 0.23309 (3) | −0.31834 (3) | 0.82278 (2) | 0.00859 (8) | |
Se2 | 0.51559 (3) | −0.44704 (3) | 0.80634 (2) | 0.01022 (8) | |
Se3 | 0.47570 (3) | 0.02579 (3) | 0.62160 (2) | 0.01098 (8) | |
Se4 | 0.36270 (3) | −0.31909 (3) | 0.66142 (2) | 0.00930 (8) | |
Se5 | 0.28008 (3) | 0.02291 (3) | 0.88460 (2) | 0.01085 (8) | |
Se6 | 0.51956 (3) | −0.09741 (3) | 0.78576 (2) | 0.00885 (8) | |
Se7 | 0.19676 (3) | −0.08788 (3) | 0.71572 (2) | 0.00948 (8) | |
Se8 | 0.00915 (3) | −0.41635 (3) | 0.67346 (2) | 0.01008 (8) | |
Fe1 | 0.42062 (4) | −0.30404 (5) | 0.77046 (2) | 0.00816 (11) | |
Fe2 | 0.18670 (4) | −0.29485 (5) | 0.71569 (2) | 0.00838 (11) | |
Fe3 | 0.39696 (4) | −0.11194 (5) | 0.69146 (2) | 0.00849 (11) | |
Fe4 | 0.30805 (4) | −0.11068 (5) | 0.80853 (2) | 0.00818 (11) | |
N1 | 0.4973 (3) | 0.8434 (3) | 0.94248 (15) | 0.0136 (7) | |
H1A | 0.448 (3) | 0.892 (3) | 0.9340 (18) | 0.016* | |
H1B | 0.490 (4) | 0.802 (3) | 0.9063 (10) | 0.016* | |
N2 | 0.6222 (3) | 0.8083 (3) | 0.57712 (14) | 0.0126 (7) | |
H2A | 0.591 (3) | 0.873 (2) | 0.5816 (18) | 0.015* | |
H2B | 0.571 (3) | 0.757 (3) | 0.5986 (16) | 0.015* | |
N3 | 0.5391 (3) | 0.2755 (3) | 0.90791 (14) | 0.0138 (7) | |
H3A | 0.534 (4) | 0.3467 (19) | 0.8947 (18) | 0.017* | |
H3B | 0.4601 (13) | 0.238 (3) | 0.9060 (19) | 0.017* | |
N4 | −0.0699 (3) | 0.8309 (3) | 0.61730 (15) | 0.0139 (7) | |
H4A | −0.026 (3) | 0.891 (2) | 0.6417 (15) | 0.017* | |
H4B | −0.039 (3) | 0.772 (3) | 0.6314 (18) | 0.017* | |
N5 | 0.1591 (3) | 0.5663 (3) | 0.52773 (15) | 0.0157 (7) | |
H5A | 0.223 (2) | 0.534 (3) | 0.5327 (19) | 0.019* | |
H5B | 0.146 (4) | 0.585 (4) | 0.5667 (7) | 0.019* | |
N7 | 0.3681 (3) | 0.5696 (3) | 0.94751 (15) | 0.0156 (7) | |
H7A | 0.425 (3) | 0.562 (4) | 0.9216 (15) | 0.019* | |
H7B | 0.313 (3) | 0.594 (4) | 0.9239 (16) | 0.019* | |
N8 | 0.2417 (3) | 1.0029 (3) | 0.32400 (15) | 0.0135 (7) | |
H8A | 0.3213 (12) | 1.006 (4) | 0.3250 (19) | 0.016* | |
H8B | 0.205 (3) | 0.982 (4) | 0.2869 (9) | 0.016* | |
N9 | 0.1297 (3) | 0.7187 (3) | 0.40169 (14) | 0.0118 (7) | |
H9A | 0.0574 (19) | 0.734 (4) | 0.4077 (18) | 0.014* | |
H9B | 0.110 (3) | 0.6404 (12) | 0.3901 (18) | 0.014* | |
N10 | −0.1535 (3) | 0.5881 (3) | 0.81593 (15) | 0.0135 (7) | |
H10A | −0.2307 (14) | 0.574 (4) | 0.8008 (17) | 0.016* | |
H10B | −0.101 (3) | 0.591 (4) | 0.7863 (13) | 0.016* | |
N12 | 0.0773 (3) | 0.1331 (3) | 0.78714 (17) | 0.0180 (8) | |
H12A | 0.134 (3) | 0.111 (4) | 0.8107 (16) | 0.022* | |
H12B | 0.063 (4) | 0.084 (3) | 0.7533 (12) | 0.022* | |
N13 | 0.2564 (3) | 0.3522 (3) | 0.86096 (15) | 0.0153 (7) | |
H13A | 0.290 (3) | 0.290 (3) | 0.8659 (19) | 0.018* | |
H13B | 0.317 (3) | 0.413 (3) | 0.8513 (19) | 0.018* | |
N14 | 0.0117 (3) | 0.4141 (3) | 0.79762 (15) | 0.0134 (7) | |
H14A | 0.000 (4) | 0.448 (3) | 0.7626 (11) | 0.016* | |
H14B | 0.064 (3) | 0.468 (3) | 0.8216 (15) | 0.016* | |
N15 | 0.4007 (3) | 0.7894 (3) | 0.49376 (15) | 0.0146 (7) | |
H15A | 0.409 (4) | 0.824 (3) | 0.5317 (8) | 0.018* | |
H15B | 0.425 (4) | 0.849 (3) | 0.4688 (16) | 0.018* | |
N16 | 0.0241 (3) | 0.7795 (3) | 0.91254 (15) | 0.0146 (7) | |
H16A | 0.077 (3) | 0.8511 (19) | 0.9124 (19) | 0.018* | |
H16B | 0.064 (3) | 0.736 (3) | 0.8897 (16) | 0.018* | |
N17 | 0.1663 (3) | 0.8433 (3) | 0.55308 (15) | 0.0163 (7) | |
H17A | 0.234 (2) | 0.898 (3) | 0.5658 (18) | 0.020* | |
H17B | 0.150 (4) | 0.802 (3) | 0.5863 (12) | 0.020* | |
N18 | 0.7145 (3) | 0.7742 (3) | 0.89574 (16) | 0.0162 (7) | |
H18A | 0.685 (4) | 0.810 (4) | 0.8649 (13) | 0.019* | |
H18B | 0.659 (3) | 0.705 (2) | 0.8959 (19) | 0.019* | |
N19 | 0.2420 (3) | 0.7809 (3) | 0.99544 (16) | 0.0174 (7) | |
H19A | 0.248 (4) | 0.814 (4) | 0.9592 (10) | 0.021* | |
H19B | 0.240 (4) | 0.842 (3) | 1.0221 (15) | 0.021* | |
N20 | −0.0885 (4) | −0.1079 (3) | 0.80260 (17) | 0.0193 (8) | |
H20A | −0.019 (4) | −0.115 (4) | 0.789 (2) | 0.023* | |
H20B | −0.142 (4) | −0.108 (4) | 0.775 (2) | 0.023* | |
N21 | 0.7131 (3) | 0.6615 (3) | 0.68026 (14) | 0.0129 (7) | |
H21A | 0.784 (2) | 0.657 (4) | 0.6988 (17) | 0.015* | |
H21B | 0.650 (2) | 0.646 (4) | 0.7040 (15) | 0.015* | |
N22 | 0.4619 (3) | 0.2194 (3) | 0.77482 (15) | 0.0156 (7) | |
H22A | 0.416 (3) | 0.152 (2) | 0.7881 (18) | 0.019* | |
H22B | 0.433 (4) | 0.280 (3) | 0.7899 (18) | 0.019* | |
N23 | 0.5410 (3) | 0.3981 (3) | 0.67015 (15) | 0.0141 (7) | |
H23A | 0.489 (3) | 0.425 (4) | 0.6460 (16) | 0.017* | |
H23B | 0.542 (4) | 0.438 (3) | 0.7062 (10) | 0.017* | |
C1 | 0.6909 (3) | 0.5686 (3) | 0.63090 (17) | 0.0123 (8) | |
H1C | 0.762564 | 0.580950 | 0.606620 | 0.015* | |
H1D | 0.623310 | 0.579231 | 0.604416 | 0.015* | |
C2 | 0.6124 (3) | 0.7679 (4) | 0.51350 (17) | 0.0177 (9) | |
H2C | 0.661928 | 0.709742 | 0.507613 | 0.021* | |
H2D | 0.645166 | 0.835994 | 0.489397 | 0.021* | |
C3 | 0.2137 (3) | 0.3794 (4) | 0.92042 (18) | 0.0173 (9) | |
H3C | 0.176491 | 0.303972 | 0.937863 | 0.021* | |
H3D | 0.150301 | 0.422983 | 0.914353 | 0.021* | |
C4 | 0.5863 (3) | 0.2379 (4) | 0.79921 (17) | 0.0136 (8) | |
H4C | 0.628153 | 0.320933 | 0.794129 | 0.016* | |
H4D | 0.626567 | 0.186916 | 0.774797 | 0.016* | |
C5 | 0.1255 (3) | 0.6950 (4) | 0.99522 (18) | 0.0180 (9) | |
H5C | 0.113172 | 0.668570 | 1.036583 | 0.022* | |
H5D | 0.128743 | 0.625057 | 0.968781 | 0.022* | |
C6 | 0.6203 (3) | 0.9169 (3) | 0.95251 (17) | 0.0140 (8) | |
H6A | 0.627267 | 0.963798 | 0.991428 | 0.017* | |
H6B | 0.637259 | 0.972722 | 0.920102 | 0.017* | |
C7 | 0.0182 (3) | 0.7406 (4) | 0.97419 (18) | 0.0175 (9) | |
H7C | −0.055347 | 0.677252 | 0.976673 | 0.021* | |
H7D | 0.011857 | 0.807642 | 1.001954 | 0.021* | |
C8 | −0.0500 (3) | 0.8437 (4) | 0.55319 (18) | 0.0155 (8) | |
H8C | −0.108237 | 0.885511 | 0.536073 | 0.019* | |
H8D | −0.066662 | 0.764026 | 0.532432 | 0.019* | |
C9 | −0.0345 (4) | 0.1159 (4) | 0.8184 (2) | 0.0183 (9) | |
H9C | −0.098390 | 0.127796 | 0.789821 | 0.022* | |
H9D | −0.024173 | 0.177812 | 0.851663 | 0.022* | |
C11 | 0.1833 (4) | 0.7927 (3) | 0.35333 (17) | 0.0151 (8) | |
H11A | 0.136081 | 0.765971 | 0.314823 | 0.018* | |
H11B | 0.265987 | 0.783963 | 0.348170 | 0.018* | |
C12 | 0.6014 (3) | 0.2127 (3) | 0.86527 (16) | 0.0121 (8) | |
H12C | 0.572022 | 0.126766 | 0.869137 | 0.015* | |
H12D | 0.687953 | 0.233809 | 0.877319 | 0.015* | |
C13 | 0.0556 (3) | 0.4759 (3) | 0.50163 (17) | 0.0119 (8) | |
H13C | 0.041653 | 0.406652 | 0.526690 | 0.014* | |
H13D | 0.072700 | 0.449422 | 0.460623 | 0.014* | |
C14 | −0.1363 (4) | 0.4963 (3) | 0.85624 (17) | 0.0143 (8) | |
H14C | −0.211055 | 0.469010 | 0.877347 | 0.017* | |
H14D | −0.072224 | 0.532640 | 0.887239 | 0.017* | |
C15 | −0.1040 (3) | 0.3892 (3) | 0.82603 (18) | 0.0143 (8) | |
H15C | −0.102545 | 0.330553 | 0.856564 | 0.017* | |
H15D | −0.167734 | 0.352795 | 0.794877 | 0.017* | |
C16 | 0.0761 (3) | 0.9104 (3) | 0.53955 (18) | 0.0153 (8) | |
H16C | 0.077291 | 0.927622 | 0.496395 | 0.018* | |
H16D | 0.096934 | 0.986740 | 0.563707 | 0.018* | |
C17 | 0.4843 (4) | 0.7115 (4) | 0.48997 (19) | 0.0207 (9) | |
H17C | 0.485777 | 0.683582 | 0.447283 | 0.025* | |
H17D | 0.453212 | 0.641405 | 0.513020 | 0.025* | |
C18 | 0.6626 (3) | 0.4420 (3) | 0.64901 (17) | 0.0132 (8) | |
H18C | 0.673124 | 0.390264 | 0.613966 | 0.016* | |
H18D | 0.721579 | 0.434751 | 0.681476 | 0.016* | |
C19 | −0.0765 (4) | −0.0038 (4) | 0.8445 (2) | 0.0218 (9) | |
H19C | −0.019529 | −0.009323 | 0.878198 | 0.026* | |
H19D | −0.155264 | −0.007029 | 0.861602 | 0.026* | |
C20 | 0.7115 (3) | 0.8423 (3) | 0.95328 (17) | 0.0142 (8) | |
H20C | 0.791911 | 0.894470 | 0.963200 | 0.017* | |
H20D | 0.693641 | 0.786626 | 0.985673 | 0.017* | |
C22 | 0.3085 (4) | 0.4515 (4) | 0.96621 (18) | 0.0179 (9) | |
H22C | 0.270339 | 0.461047 | 1.004661 | 0.021* | |
H22D | 0.370199 | 0.406516 | 0.973909 | 0.021* | |
C23 | 0.1855 (3) | 0.9217 (3) | 0.36872 (18) | 0.0134 (8) | |
H23C | 0.102221 | 0.929384 | 0.372773 | 0.016* | |
H23D | 0.229333 | 0.945997 | 0.408313 | 0.016* | |
Li1 | 0.7577 (5) | 0.8246 (6) | 0.6421 (3) | 0.0141 (14) | |
Li2 | 0.4064 (6) | 0.7262 (6) | 1.0017 (3) | 0.0162 (14) | |
Li5 | 0.2141 (5) | 0.7278 (6) | 0.4896 (3) | 0.0129 (13) | |
Li6 | −0.1309 (5) | 0.7527 (6) | 0.8581 (3) | 0.0154 (14) | |
Li4 | 0.1373 (6) | 0.3128 (6) | 0.7847 (3) | 0.0170 (14) | |
N6 | 0.2336 (6) | 0.3899 (6) | 0.71564 (18) | 0.0195 (9) | 0.935 (8) |
H6C | 0.3101 (18) | 0.383 (4) | 0.721 (2) | 0.023* | 0.935 (8) |
H6D | 0.239 (4) | 0.4674 (15) | 0.725 (2) | 0.023* | 0.935 (8) |
C10 | 0.2073 (5) | 0.3661 (4) | 0.64990 (19) | 0.0177 (10) | 0.935 (8) |
H10C | 0.277723 | 0.405388 | 0.628182 | 0.021* | 0.935 (8) |
H10D | 0.138889 | 0.399250 | 0.637314 | 0.021* | 0.935 (8) |
C21 | 0.1775 (4) | 0.2355 (4) | 0.6335 (2) | 0.0198 (11) | 0.935 (8) |
H21C | 0.106329 | 0.196734 | 0.654849 | 0.024* | 0.935 (8) |
H21D | 0.157330 | 0.221581 | 0.589634 | 0.024* | 0.935 (8) |
N24 | 0.2752 (4) | 0.1837 (4) | 0.6490 (3) | 0.0335 (13) | 0.935 (8) |
H24A | 0.276 (5) | 0.186 (5) | 0.6897 (6) | 0.040* | 0.935 (8) |
H24B | 0.271 (5) | 0.1061 (15) | 0.640 (2) | 0.040* | 0.935 (8) |
Li3 | 0.4551 (6) | 0.2192 (6) | 0.6823 (3) | 0.0170 (14) | |
N6A | 0.221 (8) | 0.375 (8) | 0.7090 (15) | 0.020 (4) | 0.065 (8) |
H6AA | 0.235880 | 0.454990 | 0.711734 | 0.024* | 0.065 (8) |
H6AB | 0.293028 | 0.354976 | 0.708873 | 0.024* | 0.065 (8) |
C10A | 0.155 (6) | 0.332 (7) | 0.6506 (16) | 0.021 (3) | 0.065 (8) |
H10E | 0.082052 | 0.271092 | 0.658274 | 0.025* | 0.065 (8) |
H10F | 0.129397 | 0.398155 | 0.632669 | 0.025* | 0.065 (8) |
C21A | 0.224 (4) | 0.280 (5) | 0.6064 (18) | 0.022 (3) | 0.065 (8) |
H21E | 0.166901 | 0.235314 | 0.574121 | 0.026* | 0.065 (8) |
H21F | 0.278237 | 0.345660 | 0.587620 | 0.026* | 0.065 (8) |
N24A | 0.294 (4) | 0.203 (5) | 0.629 (3) | 0.025 (3) | 0.065 (8) |
H24C | 0.306951 | 0.161916 | 0.595230 | 0.030* | 0.065 (8) |
H24D | 0.240096 | 0.150678 | 0.649050 | 0.030* | 0.065 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Se1 | 0.00745 (17) | 0.01009 (19) | 0.00859 (18) | 0.00206 (14) | 0.00235 (13) | 0.00248 (14) |
Se2 | 0.00890 (18) | 0.01060 (19) | 0.01223 (19) | 0.00395 (15) | 0.00204 (14) | 0.00199 (15) |
Se3 | 0.01273 (18) | 0.01107 (19) | 0.01146 (18) | 0.00579 (15) | 0.00575 (14) | 0.00452 (15) |
Se4 | 0.00803 (17) | 0.01185 (19) | 0.00829 (18) | 0.00278 (14) | 0.00216 (13) | −0.00026 (14) |
Se5 | 0.01063 (18) | 0.0120 (2) | 0.00995 (18) | 0.00294 (15) | 0.00167 (14) | −0.00080 (15) |
Se6 | 0.00723 (17) | 0.00982 (19) | 0.00919 (18) | 0.00113 (14) | 0.00079 (13) | 0.00152 (14) |
Se7 | 0.00895 (17) | 0.01200 (19) | 0.00890 (18) | 0.00486 (15) | 0.00133 (14) | 0.00209 (15) |
Se8 | 0.00716 (17) | 0.0118 (2) | 0.01137 (18) | 0.00250 (15) | −0.00047 (14) | 0.00072 (15) |
Fe1 | 0.0070 (2) | 0.0093 (3) | 0.0088 (3) | 0.0025 (2) | 0.0019 (2) | 0.0016 (2) |
Fe2 | 0.0068 (2) | 0.0102 (3) | 0.0083 (3) | 0.0021 (2) | 0.0010 (2) | 0.0007 (2) |
Fe3 | 0.0081 (2) | 0.0097 (3) | 0.0083 (3) | 0.0029 (2) | 0.0020 (2) | 0.0020 (2) |
Fe4 | 0.0081 (2) | 0.0090 (3) | 0.0078 (3) | 0.0023 (2) | 0.0014 (2) | 0.0015 (2) |
N1 | 0.0103 (16) | 0.0163 (19) | 0.0150 (17) | 0.0044 (14) | 0.0014 (13) | 0.0031 (14) |
N2 | 0.0105 (16) | 0.0159 (18) | 0.0134 (17) | 0.0074 (14) | 0.0009 (13) | 0.0005 (14) |
N3 | 0.0100 (16) | 0.0203 (19) | 0.0124 (17) | 0.0060 (14) | 0.0001 (13) | 0.0021 (14) |
N4 | 0.0136 (17) | 0.0142 (18) | 0.0149 (17) | 0.0045 (14) | 0.0004 (13) | 0.0041 (14) |
N5 | 0.0135 (17) | 0.0185 (19) | 0.0142 (17) | 0.0022 (14) | −0.0012 (14) | 0.0010 (15) |
N7 | 0.0177 (18) | 0.0172 (19) | 0.0129 (17) | 0.0050 (15) | 0.0022 (14) | 0.0036 (14) |
N8 | 0.0129 (16) | 0.0155 (18) | 0.0126 (17) | 0.0041 (14) | 0.0004 (13) | 0.0034 (14) |
N9 | 0.0103 (16) | 0.0101 (17) | 0.0144 (17) | 0.0009 (14) | 0.0015 (13) | 0.0028 (14) |
N10 | 0.0093 (16) | 0.0172 (18) | 0.0171 (18) | 0.0081 (14) | 0.0031 (13) | 0.0045 (14) |
N12 | 0.0160 (18) | 0.0123 (18) | 0.028 (2) | 0.0057 (15) | 0.0062 (15) | 0.0043 (15) |
N13 | 0.0128 (17) | 0.0168 (19) | 0.0176 (18) | 0.0045 (14) | 0.0067 (14) | 0.0053 (15) |
N14 | 0.0099 (16) | 0.0141 (18) | 0.0169 (18) | 0.0031 (14) | 0.0019 (13) | 0.0055 (14) |
N15 | 0.0120 (16) | 0.0206 (19) | 0.0119 (17) | 0.0044 (14) | 0.0017 (13) | 0.0032 (14) |
N16 | 0.0079 (16) | 0.0178 (19) | 0.0180 (18) | 0.0027 (14) | 0.0013 (13) | 0.0015 (15) |
N17 | 0.0138 (17) | 0.023 (2) | 0.0137 (17) | 0.0068 (15) | 0.0013 (14) | 0.0022 (15) |
N18 | 0.0081 (16) | 0.0187 (19) | 0.0211 (19) | 0.0029 (14) | −0.0002 (14) | −0.0029 (15) |
N19 | 0.0148 (17) | 0.021 (2) | 0.0158 (18) | 0.0020 (15) | 0.0009 (14) | 0.0042 (15) |
N20 | 0.025 (2) | 0.0123 (18) | 0.021 (2) | 0.0047 (16) | −0.0019 (16) | 0.0015 (15) |
N21 | 0.0092 (16) | 0.0157 (18) | 0.0143 (17) | 0.0036 (14) | 0.0017 (13) | 0.0028 (14) |
N22 | 0.0154 (17) | 0.0153 (19) | 0.0153 (18) | 0.0018 (14) | −0.0009 (14) | 0.0044 (14) |
N23 | 0.0164 (17) | 0.0138 (18) | 0.0118 (17) | 0.0029 (14) | 0.0005 (14) | 0.0003 (14) |
C1 | 0.0104 (18) | 0.014 (2) | 0.0123 (19) | 0.0033 (16) | 0.0016 (15) | 0.0011 (16) |
C2 | 0.0113 (19) | 0.029 (2) | 0.014 (2) | 0.0075 (18) | −0.0002 (16) | −0.0001 (18) |
C3 | 0.014 (2) | 0.020 (2) | 0.019 (2) | 0.0035 (17) | 0.0080 (16) | 0.0029 (17) |
C4 | 0.0127 (19) | 0.015 (2) | 0.014 (2) | 0.0040 (16) | 0.0027 (15) | 0.0009 (16) |
C5 | 0.018 (2) | 0.020 (2) | 0.015 (2) | 0.0017 (18) | 0.0015 (16) | 0.0050 (17) |
C6 | 0.016 (2) | 0.013 (2) | 0.0120 (19) | 0.0021 (16) | −0.0002 (15) | 0.0010 (16) |
C7 | 0.014 (2) | 0.024 (2) | 0.014 (2) | 0.0031 (17) | 0.0062 (16) | 0.0004 (17) |
C8 | 0.015 (2) | 0.014 (2) | 0.019 (2) | 0.0056 (17) | −0.0013 (16) | 0.0001 (17) |
C9 | 0.016 (2) | 0.011 (2) | 0.028 (2) | 0.0025 (17) | 0.0021 (17) | 0.0045 (18) |
C11 | 0.019 (2) | 0.014 (2) | 0.012 (2) | 0.0027 (17) | 0.0023 (16) | 0.0026 (16) |
C12 | 0.0121 (19) | 0.014 (2) | 0.0126 (19) | 0.0078 (16) | 0.0002 (15) | 0.0007 (16) |
C13 | 0.0121 (19) | 0.012 (2) | 0.0115 (19) | 0.0013 (16) | 0.0025 (15) | 0.0016 (15) |
C14 | 0.019 (2) | 0.011 (2) | 0.015 (2) | 0.0054 (16) | 0.0036 (16) | 0.0024 (16) |
C15 | 0.0102 (18) | 0.014 (2) | 0.019 (2) | 0.0027 (16) | 0.0039 (15) | 0.0031 (17) |
C16 | 0.017 (2) | 0.013 (2) | 0.017 (2) | 0.0044 (17) | 0.0036 (16) | 0.0052 (17) |
C17 | 0.016 (2) | 0.032 (3) | 0.015 (2) | 0.0097 (19) | −0.0016 (16) | −0.0083 (18) |
C18 | 0.0135 (19) | 0.013 (2) | 0.0132 (19) | 0.0050 (16) | −0.0014 (15) | −0.0001 (16) |
C19 | 0.025 (2) | 0.013 (2) | 0.029 (2) | 0.0053 (18) | 0.0082 (19) | 0.0025 (18) |
C20 | 0.0130 (19) | 0.015 (2) | 0.015 (2) | 0.0037 (16) | −0.0010 (15) | 0.0009 (16) |
C22 | 0.021 (2) | 0.018 (2) | 0.014 (2) | 0.0029 (18) | 0.0031 (16) | 0.0046 (17) |
C23 | 0.0102 (18) | 0.013 (2) | 0.017 (2) | 0.0028 (16) | 0.0012 (15) | 0.0023 (16) |
Li1 | 0.009 (3) | 0.017 (4) | 0.018 (3) | 0.006 (3) | −0.001 (3) | 0.004 (3) |
Li2 | 0.015 (3) | 0.020 (4) | 0.013 (3) | 0.002 (3) | 0.001 (3) | 0.003 (3) |
Li5 | 0.011 (3) | 0.016 (3) | 0.010 (3) | 0.001 (3) | −0.001 (2) | 0.000 (3) |
Li6 | 0.007 (3) | 0.015 (4) | 0.023 (4) | 0.002 (3) | 0.000 (3) | −0.003 (3) |
Li4 | 0.011 (3) | 0.014 (4) | 0.025 (3) | 0.001 (3) | 0.001 (3) | −0.002 (3) |
N6 | 0.020 (2) | 0.019 (3) | 0.0166 (19) | −0.0016 (17) | 0.0021 (17) | −0.0056 (17) |
C10 | 0.013 (2) | 0.020 (2) | 0.021 (2) | 0.0058 (18) | −0.0039 (17) | 0.0005 (18) |
C21 | 0.019 (2) | 0.020 (2) | 0.021 (2) | 0.0077 (18) | −0.0066 (18) | −0.0024 (18) |
N24 | 0.015 (2) | 0.015 (2) | 0.072 (3) | 0.0062 (17) | −0.001 (2) | 0.007 (2) |
Li3 | 0.017 (3) | 0.016 (4) | 0.020 (4) | 0.008 (3) | 0.001 (3) | −0.002 (3) |
N6A | 0.017 (6) | 0.019 (6) | 0.022 (5) | 0.002 (6) | −0.002 (5) | −0.002 (5) |
C10A | 0.017 (5) | 0.019 (5) | 0.025 (4) | 0.004 (5) | −0.005 (4) | −0.003 (5) |
C21A | 0.016 (5) | 0.017 (5) | 0.034 (5) | 0.007 (4) | −0.004 (5) | 0.001 (5) |
N24A | 0.018 (6) | 0.017 (6) | 0.041 (6) | 0.006 (5) | −0.004 (6) | 0.005 (6) |
Se1—Fe1 | 2.4674 (7) | N21—H21A | 0.909 (10) |
Se1—Fe2 | 2.4611 (8) | N21—H21B | 0.908 (10) |
Se1—Fe4 | 2.4157 (8) | N21—C1 | 1.473 (5) |
Se2—Fe1 | 2.3502 (7) | N21—Li1 | 2.084 (7) |
Se3—Fe3 | 2.3456 (7) | N22—H22A | 0.905 (10) |
Se3—Li3 | 2.634 (7) | N22—H22B | 0.907 (10) |
Se4—Fe1 | 2.4739 (8) | N22—C4 | 1.471 (5) |
Se4—Fe2 | 2.4629 (7) | N22—Li3 | 2.055 (8) |
Se4—Fe3 | 2.4108 (8) | N23—H23A | 0.906 (10) |
Se5—Fe4 | 2.3251 (8) | N23—H23B | 0.906 (10) |
Se6—Fe1 | 2.4133 (8) | N23—C18 | 1.477 (5) |
Se6—Fe3 | 2.4531 (8) | N23—Li3 | 2.126 (8) |
Se6—Fe4 | 2.4752 (8) | C1—H1C | 0.9900 |
Se7—Fe2 | 2.3899 (8) | C1—H1D | 0.9900 |
Se7—Fe3 | 2.4608 (8) | C1—C18 | 1.516 (5) |
Se7—Fe4 | 2.4414 (7) | C2—H2C | 0.9900 |
Se8—Fe2 | 2.3262 (7) | C2—H2D | 0.9900 |
Fe1—Fe2 | 2.9327 (9) | C2—C17 | 1.524 (5) |
Fe1—Fe3 | 2.9702 (9) | C3—H3C | 0.9900 |
Fe1—Fe4 | 2.9566 (9) | C3—H3D | 0.9900 |
Fe2—Fe3 | 2.9154 (9) | C3—C22 | 1.524 (6) |
Fe2—Fe4 | 2.9556 (9) | C4—H4C | 0.9900 |
Fe3—Fe4 | 2.8362 (9) | C4—H4D | 0.9900 |
N1—H1A | 0.907 (10) | C4—C12 | 1.523 (5) |
N1—H1B | 0.908 (10) | C5—H5C | 0.9900 |
N1—C6 | 1.474 (5) | C5—H5D | 0.9900 |
N1—Li2 | 2.079 (7) | C5—C7 | 1.519 (5) |
N2—H2A | 0.907 (10) | C6—H6A | 0.9900 |
N2—H2B | 0.907 (10) | C6—H6B | 0.9900 |
N2—C2 | 1.460 (5) | C6—C20 | 1.511 (5) |
N2—Li1 | 2.049 (7) | C7—H7C | 0.9900 |
N3—H3A | 0.909 (10) | C7—H7D | 0.9900 |
N3—H3B | 0.909 (10) | C8—H8C | 0.9900 |
N3—C12 | 1.476 (5) | C8—H8D | 0.9900 |
N3—Li2i | 2.082 (7) | C8—C16 | 1.527 (5) |
N4—H4A | 0.906 (10) | C9—H9C | 0.9900 |
N4—H4B | 0.907 (10) | C9—H9D | 0.9900 |
N4—C8 | 1.463 (5) | C9—C19 | 1.519 (5) |
N4—Li1ii | 2.065 (7) | C11—H11A | 0.9900 |
N5—H5A | 0.908 (10) | C11—H11B | 0.9900 |
N5—H5B | 0.908 (10) | C11—C23 | 1.521 (5) |
N5—C13 | 1.470 (5) | C12—H12C | 0.9900 |
N5—Li5 | 2.077 (7) | C12—H12D | 0.9900 |
N7—H7A | 0.907 (10) | C13—C13vi | 1.513 (7) |
N7—H7B | 0.908 (10) | C13—H13C | 0.9900 |
N7—C22 | 1.477 (5) | C13—H13D | 0.9900 |
N7—Li2 | 2.085 (8) | C14—H14C | 0.9900 |
N8—H8A | 0.907 (10) | C14—H14D | 0.9900 |
N8—H8B | 0.906 (10) | C14—C15 | 1.518 (5) |
N8—C23 | 1.471 (5) | C15—H15C | 0.9900 |
N8—Li1iii | 2.111 (8) | C15—H15D | 0.9900 |
N9—H9A | 0.906 (10) | C16—H16C | 0.9900 |
N9—H9B | 0.910 (10) | C16—H16D | 0.9900 |
N9—C11 | 1.476 (5) | C17—H17C | 0.9900 |
N9—Li5 | 2.133 (7) | C17—H17D | 0.9900 |
N10—H10A | 0.909 (7) | C18—H18C | 0.9900 |
N10—H10B | 0.910 (7) | C18—H18D | 0.9900 |
N10—C14 | 1.474 (5) | C19—H19C | 0.9900 |
N10—Li6 | 2.049 (8) | C19—H19D | 0.9900 |
N12—H12A | 0.905 (10) | C20—H20C | 0.9900 |
N12—H12B | 0.908 (10) | C20—H20D | 0.9900 |
N12—C9 | 1.464 (5) | C22—H22C | 0.9900 |
N12—Li4 | 2.052 (8) | C22—H22D | 0.9900 |
N13—H13A | 0.908 (10) | C23—H23C | 0.9900 |
N13—H13B | 0.908 (10) | C23—H23D | 0.9900 |
N13—C3 | 1.474 (5) | Li1—H2B | 2.26 (4) |
N13—Li4 | 2.097 (8) | Li2—H7B | 2.31 (4) |
N14—H14A | 0.908 (10) | Li4—H14B | 2.30 (4) |
N14—H14B | 0.902 (10) | Li4—N6 | 2.051 (8) |
N14—C15 | 1.469 (5) | Li4—N6A | 2.05 (2) |
N14—Li4 | 2.088 (7) | N6—H6C | 0.907 (10) |
N15—H15A | 0.909 (10) | N6—H6D | 0.903 (10) |
N15—H15B | 0.909 (10) | N6—C10 | 1.479 (6) |
N15—C17 | 1.470 (5) | C10—H10C | 0.9900 |
N15—Li5 | 2.094 (7) | C10—H10D | 0.9900 |
N16—H16A | 0.909 (10) | C10—C21 | 1.504 (6) |
N16—H16B | 0.908 (10) | C21—H21C | 0.9900 |
N16—C7 | 1.465 (5) | C21—H21D | 0.9900 |
N16—Li6 | 2.064 (7) | C21—N24 | 1.431 (6) |
N17—H17A | 0.907 (10) | N24—H24A | 0.902 (10) |
N17—H17B | 0.908 (10) | N24—H24B | 0.906 (10) |
N17—C16 | 1.468 (5) | N24—Li3 | 2.107 (8) |
N17—Li5 | 2.080 (7) | Li3—H24A | 2.01 (6) |
N18—H18A | 0.909 (10) | Li3—N24A | 2.12 (2) |
N18—H18B | 0.907 (10) | N6A—H6AA | 0.9100 |
N18—C20 | 1.477 (5) | N6A—H6AB | 0.9100 |
N18—Li6iv | 2.058 (7) | N6A—C10A | 1.48 (2) |
N19—H19A | 0.910 (10) | C10A—H10E | 0.9900 |
N19—H19B | 0.907 (10) | C10A—H10F | 0.9900 |
N19—C5 | 1.472 (5) | C10A—C21A | 1.48 (2) |
N19—Li2 | 2.133 (7) | C21A—H21E | 0.9900 |
N20—H20A | 0.89 (5) | C21A—H21F | 0.9900 |
N20—H20B | 0.85 (5) | C21A—N24A | 1.44 (2) |
N20—C19 | 1.469 (6) | N24A—H24C | 0.9100 |
N20—Li6v | 2.070 (7) | N24A—H24D | 0.9100 |
Fe2—Se1—Fe1 | 73.03 (2) | C18—C1—H1D | 108.1 |
Fe4—Se1—Fe1 | 74.52 (2) | N2—C2—H2C | 108.9 |
Fe4—Se1—Fe2 | 74.60 (2) | N2—C2—H2D | 108.9 |
Fe3—Se3—Li3 | 98.63 (15) | N2—C2—C17 | 113.6 (3) |
Fe2—Se4—Fe1 | 72.89 (2) | H2C—C2—H2D | 107.7 |
Fe3—Se4—Fe1 | 74.89 (2) | C17—C2—H2C | 108.9 |
Fe3—Se4—Fe2 | 73.47 (2) | C17—C2—H2D | 108.9 |
Fe1—Se6—Fe3 | 75.23 (2) | N13—C3—H3C | 108.3 |
Fe1—Se6—Fe4 | 74.42 (2) | N13—C3—H3D | 108.3 |
Fe3—Se6—Fe4 | 70.27 (2) | N13—C3—C22 | 115.9 (3) |
Fe2—Se7—Fe3 | 73.87 (2) | H3C—C3—H3D | 107.4 |
Fe2—Se7—Fe4 | 75.43 (2) | C22—C3—H3C | 108.3 |
Fe4—Se7—Fe3 | 70.70 (2) | C22—C3—H3D | 108.3 |
Se1—Fe1—Se4 | 105.83 (3) | N22—C4—H4C | 108.4 |
Se1—Fe1—Fe2 | 53.39 (2) | N22—C4—H4D | 108.4 |
Se1—Fe1—Fe3 | 97.87 (2) | N22—C4—C12 | 115.7 (3) |
Se1—Fe1—Fe4 | 51.944 (18) | H4C—C4—H4D | 107.4 |
Se2—Fe1—Se1 | 108.31 (2) | C12—C4—H4C | 108.4 |
Se2—Fe1—Se4 | 117.08 (3) | C12—C4—H4D | 108.4 |
Se2—Fe1—Se6 | 119.59 (3) | N19—C5—H5C | 108.5 |
Se2—Fe1—Fe2 | 138.02 (3) | N19—C5—H5D | 108.5 |
Se2—Fe1—Fe3 | 153.78 (3) | N19—C5—C7 | 115.1 (3) |
Se2—Fe1—Fe4 | 143.63 (3) | H5C—C5—H5D | 107.5 |
Se4—Fe1—Fe2 | 53.381 (17) | C7—C5—H5C | 108.5 |
Se4—Fe1—Fe3 | 51.589 (19) | C7—C5—H5D | 108.5 |
Se4—Fe1—Fe4 | 98.75 (2) | N1—C6—H6A | 109.3 |
Se6—Fe1—Se1 | 103.23 (2) | N1—C6—H6B | 109.3 |
Se6—Fe1—Se4 | 101.23 (2) | N1—C6—C20 | 111.5 (3) |
Se6—Fe1—Fe2 | 102.13 (2) | H6A—C6—H6B | 108.0 |
Se6—Fe1—Fe3 | 53.00 (2) | C20—C6—H6A | 109.3 |
Se6—Fe1—Fe4 | 53.75 (2) | C20—C6—H6B | 109.3 |
Fe2—Fe1—Fe3 | 59.189 (18) | N16—C7—C5 | 113.9 (3) |
Fe2—Fe1—Fe4 | 60.25 (2) | N16—C7—H7C | 108.8 |
Fe4—Fe1—Fe3 | 57.18 (2) | N16—C7—H7D | 108.8 |
Se1—Fe2—Se4 | 106.37 (2) | C5—C7—H7C | 108.8 |
Se1—Fe2—Fe1 | 53.582 (17) | C5—C7—H7D | 108.8 |
Se1—Fe2—Fe3 | 99.46 (2) | H7C—C7—H7D | 107.7 |
Se1—Fe2—Fe4 | 52.00 (2) | N4—C8—H8C | 108.6 |
Se4—Fe2—Fe1 | 53.73 (2) | N4—C8—H8D | 108.6 |
Se4—Fe2—Fe3 | 52.44 (2) | N4—C8—C16 | 114.7 (3) |
Se4—Fe2—Fe4 | 99.03 (2) | H8C—C8—H8D | 107.6 |
Se7—Fe2—Se1 | 101.70 (2) | C16—C8—H8C | 108.6 |
Se7—Fe2—Se4 | 104.06 (2) | C16—C8—H8D | 108.6 |
Se7—Fe2—Fe1 | 103.32 (2) | N12—C9—H9C | 108.4 |
Se7—Fe2—Fe3 | 54.18 (2) | N12—C9—H9D | 108.4 |
Se7—Fe2—Fe4 | 53.076 (19) | N12—C9—C19 | 115.6 (3) |
Se8—Fe2—Se1 | 116.00 (2) | H9C—C9—H9D | 107.4 |
Se8—Fe2—Se4 | 112.40 (3) | C19—C9—H9C | 108.4 |
Se8—Fe2—Se7 | 115.01 (3) | C19—C9—H9D | 108.4 |
Se8—Fe2—Fe1 | 141.65 (3) | N9—C11—H11A | 109.6 |
Se8—Fe2—Fe3 | 144.53 (3) | N9—C11—H11B | 109.6 |
Se8—Fe2—Fe4 | 148.55 (3) | N9—C11—C23 | 110.4 (3) |
Fe1—Fe2—Fe4 | 60.28 (2) | H11A—C11—H11B | 108.1 |
Fe3—Fe2—Fe1 | 61.05 (2) | C23—C11—H11A | 109.6 |
Fe3—Fe2—Fe4 | 57.77 (2) | C23—C11—H11B | 109.6 |
Se3—Fe3—Se4 | 118.26 (3) | N3—C12—C4 | 115.6 (3) |
Se3—Fe3—Se6 | 114.85 (3) | N3—C12—H12C | 108.4 |
Se3—Fe3—Se7 | 108.75 (2) | N3—C12—H12D | 108.4 |
Se3—Fe3—Fe1 | 150.72 (3) | C4—C12—H12C | 108.4 |
Se3—Fe3—Fe2 | 143.27 (3) | C4—C12—H12D | 108.4 |
Se3—Fe3—Fe4 | 137.92 (3) | H12C—C12—H12D | 107.4 |
Se4—Fe3—Se6 | 101.90 (2) | N5—C13—C13vi | 110.8 (4) |
Se4—Fe3—Se7 | 103.50 (2) | N5—C13—H13C | 109.5 |
Se4—Fe3—Fe1 | 53.52 (2) | N5—C13—H13D | 109.5 |
Se4—Fe3—Fe2 | 54.084 (19) | C13vi—C13—H13C | 109.5 |
Se4—Fe3—Fe4 | 103.67 (2) | C13vi—C13—H13D | 109.5 |
Se6—Fe3—Se7 | 108.66 (3) | H13C—C13—H13D | 108.1 |
Se6—Fe3—Fe1 | 51.778 (19) | N10—C14—H14C | 108.3 |
Se6—Fe3—Fe2 | 101.62 (2) | N10—C14—H14D | 108.3 |
Se6—Fe3—Fe4 | 55.23 (2) | N10—C14—C15 | 115.8 (3) |
Se7—Fe3—Fe1 | 100.50 (2) | H14C—C14—H14D | 107.4 |
Se7—Fe3—Fe2 | 51.95 (2) | C15—C14—H14C | 108.3 |
Se7—Fe3—Fe4 | 54.331 (17) | C15—C14—H14D | 108.3 |
Fe2—Fe3—Fe1 | 59.76 (2) | N14—C15—C14 | 114.8 (3) |
Fe4—Fe3—Fe1 | 61.17 (2) | N14—C15—H15C | 108.6 |
Fe4—Fe3—Fe2 | 61.83 (2) | N14—C15—H15D | 108.6 |
Se1—Fe4—Se6 | 102.93 (2) | C14—C15—H15C | 108.6 |
Se1—Fe4—Se7 | 101.53 (2) | C14—C15—H15D | 108.6 |
Se1—Fe4—Fe1 | 53.54 (2) | H15C—C15—H15D | 107.5 |
Se1—Fe4—Fe2 | 53.40 (2) | N17—C16—C8 | 112.3 (3) |
Se1—Fe4—Fe3 | 102.80 (2) | N17—C16—H16C | 109.1 |
Se5—Fe4—Se1 | 117.39 (3) | N17—C16—H16D | 109.1 |
Se5—Fe4—Se6 | 114.88 (3) | C8—C16—H16C | 109.1 |
Se5—Fe4—Se7 | 110.38 (3) | C8—C16—H16D | 109.1 |
Se5—Fe4—Fe1 | 148.27 (3) | H16C—C16—H16D | 107.9 |
Se5—Fe4—Fe2 | 144.99 (3) | N15—C17—C2 | 115.0 (4) |
Se5—Fe4—Fe3 | 139.68 (3) | N15—C17—H17C | 108.5 |
Se6—Fe4—Fe1 | 51.836 (18) | N15—C17—H17D | 108.5 |
Se6—Fe4—Fe2 | 99.98 (2) | C2—C17—H17C | 108.5 |
Se6—Fe4—Fe3 | 54.502 (17) | C2—C17—H17D | 108.5 |
Se7—Fe4—Se6 | 108.57 (3) | H17C—C17—H17D | 107.5 |
Se7—Fe4—Fe1 | 101.35 (2) | N23—C18—C1 | 115.2 (3) |
Se7—Fe4—Fe2 | 51.50 (2) | N23—C18—H18C | 108.5 |
Se7—Fe4—Fe3 | 54.97 (2) | N23—C18—H18D | 108.5 |
Fe2—Fe4—Fe1 | 59.48 (2) | C1—C18—H18C | 108.5 |
Fe3—Fe4—Fe1 | 61.652 (19) | C1—C18—H18D | 108.5 |
Fe3—Fe4—Fe2 | 60.40 (2) | H18C—C18—H18D | 107.5 |
H1A—N1—H1B | 99 (4) | N20—C19—C9 | 116.5 (4) |
C6—N1—H1A | 108 (3) | N20—C19—H19C | 108.2 |
C6—N1—H1B | 109 (3) | N20—C19—H19D | 108.2 |
C6—N1—Li2 | 126.1 (3) | C9—C19—H19C | 108.2 |
Li2—N1—H1A | 105 (3) | C9—C19—H19D | 108.2 |
Li2—N1—H1B | 106 (3) | H19C—C19—H19D | 107.3 |
H2A—N2—H2B | 100 (4) | N18—C20—C6 | 114.0 (3) |
C2—N2—H2A | 109 (3) | N18—C20—H20C | 108.8 |
C2—N2—H2B | 111 (3) | N18—C20—H20D | 108.8 |
C2—N2—Li1 | 131.7 (3) | C6—C20—H20C | 108.8 |
Li1—N2—H2A | 108 (3) | C6—C20—H20D | 108.8 |
Li1—N2—H2B | 92 (3) | H20C—C20—H20D | 107.7 |
H3A—N3—H3B | 100 (4) | N7—C22—C3 | 114.5 (3) |
C12—N3—H3A | 111 (3) | N7—C22—H22C | 108.6 |
C12—N3—H3B | 109 (3) | N7—C22—H22D | 108.6 |
C12—N3—Li2i | 114.9 (3) | C3—C22—H22C | 108.6 |
Li2i—N3—H3A | 116 (3) | C3—C22—H22D | 108.6 |
Li2i—N3—H3B | 104 (3) | H22C—C22—H22D | 107.6 |
H4A—N4—H4B | 98 (4) | N8—C23—C11 | 114.3 (3) |
C8—N4—H4A | 114 (3) | N8—C23—H23C | 108.7 |
C8—N4—H4B | 111 (3) | N8—C23—H23D | 108.7 |
C8—N4—Li1ii | 115.7 (3) | C11—C23—H23C | 108.7 |
Li1ii—N4—H4A | 102 (3) | C11—C23—H23D | 108.7 |
Li1ii—N4—H4B | 114 (3) | H23C—C23—H23D | 107.6 |
H5A—N5—H5B | 101 (4) | N2—Li1—H2B | 23.6 (5) |
C13—N5—H5A | 110 (3) | N2—Li1—N4iv | 119.8 (3) |
C13—N5—H5B | 109 (3) | N2—Li1—N8iii | 97.3 (3) |
C13—N5—Li5 | 121.3 (3) | N2—Li1—N21 | 102.0 (3) |
Li5—N5—H5A | 109 (3) | N4iv—Li1—H2B | 136.0 (10) |
Li5—N5—H5B | 105 (3) | N4iv—Li1—N8iii | 105.9 (3) |
H7A—N7—H7B | 103 (4) | N4iv—Li1—N21 | 101.7 (3) |
C22—N7—H7A | 109 (3) | N8iii—Li1—H2B | 103.6 (11) |
C22—N7—H7B | 106 (3) | N21—Li1—H2B | 81.1 (7) |
C22—N7—Li2 | 126.1 (3) | N21—Li1—N8iii | 132.1 (3) |
Li2—N7—H7A | 115 (3) | N1—Li2—N3i | 123.8 (4) |
Li2—N7—H7B | 93 (3) | N1—Li2—N7 | 100.6 (3) |
H8A—N8—H8B | 113 (4) | N1—Li2—H7B | 92.4 (10) |
C23—N8—H8A | 109 (3) | N1—Li2—N19 | 96.7 (3) |
C23—N8—H8B | 111 (3) | N3i—Li2—N7 | 119.6 (3) |
C23—N8—Li1iii | 106.9 (3) | N3i—Li2—H7B | 138.6 (9) |
Li1iii—N8—H8A | 101 (3) | N3i—Li2—N19 | 109.5 (3) |
Li1iii—N8—H8B | 115 (3) | N7—Li2—H7B | 23.1 (5) |
H9A—N9—H9B | 103 (4) | N7—Li2—N19 | 102.7 (3) |
C11—N9—H9A | 107 (3) | N19—Li2—H7B | 82.3 (7) |
C11—N9—H9B | 113 (3) | N5—Li5—N9 | 109.6 (3) |
C11—N9—Li5 | 122.9 (3) | N5—Li5—N15 | 112.6 (3) |
Li5—N9—H9A | 105 (3) | N5—Li5—N17 | 102.1 (3) |
Li5—N9—H9B | 105 (3) | N15—Li5—N9 | 114.8 (3) |
H10A—N10—H10B | 112 (4) | N17—Li5—N9 | 115.7 (3) |
C14—N10—H10A | 112 (3) | N17—Li5—N15 | 101.2 (3) |
C14—N10—H10B | 108 (3) | N10—Li6—N16 | 106.0 (3) |
C14—N10—Li6 | 114.3 (3) | N10—Li6—N18ii | 111.6 (3) |
Li6—N10—H10A | 101 (3) | N10—Li6—N20vii | 115.3 (3) |
Li6—N10—H10B | 109 (3) | N16—Li6—N20vii | 101.4 (3) |
H12A—N12—H12B | 108 (4) | N18ii—Li6—N16 | 118.9 (4) |
C9—N12—H12A | 109 (3) | N18ii—Li6—N20vii | 103.7 (3) |
C9—N12—H12B | 107 (3) | N12—Li4—N13 | 101.3 (3) |
C9—N12—Li4 | 105.0 (3) | N12—Li4—N14 | 117.0 (3) |
Li4—N12—H12A | 104 (3) | N12—Li4—H14B | 132.6 (10) |
Li4—N12—H12B | 123 (3) | N12—Li4—N6A | 117 (3) |
H13A—N13—H13B | 105 (4) | N13—Li4—H14B | 84.9 (7) |
C3—N13—H13A | 106 (3) | N14—Li4—N13 | 105.8 (3) |
C3—N13—H13B | 110 (3) | N14—Li4—H14B | 23.1 (5) |
C3—N13—Li4 | 120.5 (3) | N6—Li4—N12 | 122.4 (4) |
Li4—N13—H13A | 109 (3) | N6—Li4—N13 | 105.0 (3) |
Li4—N13—H13B | 106 (3) | N6—Li4—N14 | 103.6 (4) |
H14A—N14—H14B | 107 (4) | N6—Li4—H14B | 100.2 (11) |
C15—N14—H14A | 107 (3) | N6A—Li4—N13 | 111 (2) |
C15—N14—H14B | 108 (3) | N6A—Li4—N14 | 104 (4) |
C15—N14—Li4 | 131.9 (3) | N6A—Li4—H14B | 104 (3) |
Li4—N14—H14A | 108 (3) | Li4—N6—H6C | 108 (3) |
Li4—N14—H14B | 92 (3) | Li4—N6—H6D | 102 (3) |
H15A—N15—H15B | 106 (4) | H6C—N6—H6D | 103 (4) |
C17—N15—H15A | 108 (3) | C10—N6—Li4 | 128.5 (4) |
C17—N15—H15B | 108 (3) | C10—N6—H6C | 104 (3) |
C17—N15—Li5 | 123.7 (3) | C10—N6—H6D | 109 (3) |
Li5—N15—H15A | 98 (3) | N6—C10—H10C | 109.5 |
Li5—N15—H15B | 112 (3) | N6—C10—H10D | 109.5 |
H16A—N16—H16B | 99 (4) | N6—C10—C21 | 110.7 (4) |
C7—N16—H16A | 109 (3) | H10C—C10—H10D | 108.1 |
C7—N16—H16B | 110 (3) | C21—C10—H10C | 109.5 |
C7—N16—Li6 | 119.8 (3) | C21—C10—H10D | 109.5 |
Li6—N16—H16A | 117 (3) | C10—C21—H21C | 109.3 |
Li6—N16—H16B | 98 (3) | C10—C21—H21D | 109.3 |
H17A—N17—H17B | 102 (4) | H21C—C21—H21D | 107.9 |
C16—N17—H17A | 106 (3) | N24—C21—C10 | 111.8 (4) |
C16—N17—H17B | 112 (3) | N24—C21—H21C | 109.3 |
C16—N17—Li5 | 122.6 (3) | N24—C21—H21D | 109.3 |
Li5—N17—H17A | 107 (3) | C21—N24—H24A | 103 (4) |
Li5—N17—H17B | 105 (3) | C21—N24—H24B | 121 (4) |
H18A—N18—H18B | 102 (4) | C21—N24—Li3 | 144.7 (4) |
C20—N18—H18A | 110 (3) | H24A—N24—H24B | 101 (5) |
C20—N18—H18B | 108 (3) | Li3—N24—H24A | 72 (4) |
C20—N18—Li6iv | 124.2 (3) | Li3—N24—H24B | 94 (4) |
Li6iv—N18—H18A | 98 (3) | Se3—Li3—H24A | 100.9 (15) |
Li6iv—N18—H18B | 112 (3) | N22—Li3—Se3 | 117.6 (3) |
H19A—N19—H19B | 104 (4) | N22—Li3—N23 | 100.7 (3) |
C5—N19—H19A | 109 (3) | N22—Li3—N24 | 109.6 (4) |
C5—N19—H19B | 108 (3) | N22—Li3—H24A | 84.5 (5) |
C5—N19—Li2 | 121.3 (3) | N22—Li3—N24A | 123 (2) |
Li2—N19—H19A | 100 (3) | N23—Li3—Se3 | 129.2 (3) |
Li2—N19—H19B | 113 (3) | N23—Li3—H24A | 115.6 (17) |
H20A—N20—H20B | 114 (4) | N24—Li3—Se3 | 88.4 (3) |
C19—N20—H20A | 113 (3) | N24—Li3—N23 | 109.9 (3) |
C19—N20—H20B | 109 (3) | N24—Li3—H24A | 25.2 (4) |
C19—N20—Li6v | 103.1 (3) | N24A—Li3—Se3 | 86.1 (15) |
Li6v—N20—H20A | 103 (3) | N24A—Li3—N23 | 100.3 (16) |
Li6v—N20—H20B | 114 (3) | Li4—N6A—H6AA | 108.3 |
H21A—N21—H21B | 114 (4) | Li4—N6A—H6AB | 108.3 |
C1—N21—H21A | 104 (3) | H6AA—N6A—H6AB | 107.4 |
C1—N21—H21B | 107 (3) | C10A—N6A—Li4 | 116 (3) |
C1—N21—Li1 | 107.9 (3) | C10A—N6A—H6AA | 108.3 |
Li1—N21—H21A | 103 (3) | C10A—N6A—H6AB | 108.3 |
Li1—N21—H21B | 119 (3) | N6A—C10A—H10E | 108.6 |
H22A—N22—H22B | 107 (4) | N6A—C10A—H10F | 108.6 |
C4—N22—H22A | 110 (3) | H10E—C10A—H10F | 107.5 |
C4—N22—H22B | 107 (3) | C21A—C10A—N6A | 115 (3) |
C4—N22—Li3 | 110.9 (3) | C21A—C10A—H10E | 108.6 |
Li3—N22—H22A | 112 (3) | C21A—C10A—H10F | 108.6 |
Li3—N22—H22B | 109 (3) | C10A—C21A—H21E | 108.2 |
H23A—N23—H23B | 104 (4) | C10A—C21A—H21F | 108.2 |
C18—N23—H23A | 108 (3) | H21E—C21A—H21F | 107.3 |
C18—N23—H23B | 105 (3) | N24A—C21A—C10A | 116 (3) |
C18—N23—Li3 | 126.5 (3) | N24A—C21A—H21E | 108.2 |
Li3—N23—H23A | 105 (3) | N24A—C21A—H21F | 108.2 |
Li3—N23—H23B | 107 (3) | Li3—N24A—H24C | 102.7 |
N21—C1—H1C | 108.1 | Li3—N24A—H24D | 102.7 |
N21—C1—H1D | 108.1 | C21A—N24A—Li3 | 138 (3) |
N21—C1—C18 | 116.6 (3) | C21A—N24A—H24C | 102.7 |
H1C—C1—H1D | 107.3 | C21A—N24A—H24D | 102.7 |
C18—C1—H1C | 108.1 | H24C—N24A—H24D | 105.0 |
N1—C6—C20—N18 | 62.8 (4) | Li5—N9—C11—C23 | −67.9 (4) |
N2—C2—C17—N15 | 60.7 (5) | Li5—N15—C17—C2 | −161.3 (3) |
N4—C8—C16—N17 | 69.1 (4) | Li5—N17—C16—C8 | 90.2 (4) |
N9—C11—C23—N8 | 177.8 (3) | Li6—N10—C14—C15 | −157.0 (3) |
N10—C14—C15—N14 | 63.8 (5) | Li6—N16—C7—C5 | 144.6 (4) |
N12—C9—C19—N20 | −53.8 (5) | Li6iv—N18—C20—C6 | 139.2 (4) |
N13—C3—C22—N7 | 60.9 (5) | Li6v—N20—C19—C9 | 174.9 (3) |
N19—C5—C7—N16 | 59.9 (5) | Li4—N12—C9—C19 | −160.7 (4) |
N21—C1—C18—N23 | 74.6 (4) | Li4—N13—C3—C22 | −157.0 (3) |
N22—C4—C12—N3 | −54.0 (5) | Li4—N14—C15—C14 | 148.6 (4) |
Li1—N2—C2—C17 | 150.7 (4) | Li4—N6—C10—C21 | −48.1 (9) |
Li1ii—N4—C8—C16 | 149.4 (3) | Li4—N6A—C10A—C21A | −128 (6) |
Li1iii—N8—C23—C11 | −176.9 (3) | N6—C10—C21—N24 | −61.0 (6) |
Li1—N21—C1—C18 | 177.2 (3) | C10—C21—N24—Li3 | −5.6 (10) |
Li2—N1—C6—C20 | 67.1 (5) | Li3—N22—C4—C12 | −166.9 (3) |
Li2i—N3—C12—C4 | −165.5 (3) | Li3—N23—C18—C1 | 166.7 (3) |
Li2—N7—C22—C3 | 136.6 (4) | N6A—C10A—C21A—N24A | 43 (9) |
Li2—N19—C5—C7 | −164.6 (3) | C10A—C21A—N24A—Li3 | −74 (8) |
Li5—N5—C13—C13vi | −57.2 (5) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) x−1, y, z; (iii) −x+1, −y+2, −z+1; (iv) x+1, y, z; (v) x, y−1, z; (vi) −x, −y+1, −z+1; (vii) x, y+1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Se5vii | 0.91 (1) | 2.94 (1) | 3.837 (3) | 169 (4) |
N1—H1B···Se6vii | 0.91 (1) | 2.98 (3) | 3.594 (3) | 127 (3) |
N2—H2A···Se3vii | 0.91 (1) | 2.60 (2) | 3.483 (3) | 163 (3) |
N2—H2B···Se4vii | 0.91 (1) | 2.81 (2) | 3.646 (3) | 155 (3) |
N3—H3B···Se5 | 0.91 (1) | 2.86 (2) | 3.665 (4) | 148 (3) |
N4—H4A···Se7vii | 0.91 (1) | 2.94 (3) | 3.600 (3) | 131 (3) |
N4—H4B···Se8vii | 0.91 (1) | 2.60 (1) | 3.493 (3) | 170 (4) |
N5—H5B···Se4vii | 0.91 (1) | 3.15 (4) | 3.696 (3) | 121 (3) |
N5—H5B···Se8vii | 0.91 (1) | 2.90 (2) | 3.751 (3) | 156 (4) |
N7—H7A···Se2vii | 0.91 (1) | 2.81 (2) | 3.647 (3) | 154 (3) |
N7—H7B···Se1vii | 0.91 (1) | 2.73 (2) | 3.573 (3) | 155 (3) |
N8—H8A···Se3viii | 0.91 (1) | 2.68 (2) | 3.514 (3) | 152 (3) |
N9—H9B···Se8ix | 0.91 (1) | 2.92 (2) | 3.786 (3) | 161 (3) |
N10—H10A···Se2x | 0.91 (1) | 2.88 (2) | 3.725 (3) | 156 (3) |
N10—H10B···Se8vii | 0.91 (1) | 2.86 (1) | 3.749 (3) | 165 (3) |
N12—H12A···Se5 | 0.91 (1) | 2.71 (1) | 3.611 (4) | 173 (4) |
N12—H12B···Se7 | 0.91 (1) | 2.91 (4) | 3.532 (3) | 127 (3) |
N13—H13A···Se5 | 0.91 (1) | 3.14 (2) | 3.973 (4) | 153 (3) |
N13—H13B···Se2vii | 0.91 (1) | 2.74 (2) | 3.628 (3) | 166 (4) |
N14—H14A···Se8vii | 0.91 (1) | 2.59 (1) | 3.479 (3) | 166 (4) |
N14—H14B···Se1vii | 0.90 (1) | 2.77 (3) | 3.539 (3) | 144 (3) |
N15—H15A···Se3vii | 0.91 (1) | 2.94 (2) | 3.785 (4) | 154 (3) |
N15—H15B···Se3viii | 0.91 (1) | 2.68 (2) | 3.560 (3) | 163 (4) |
N16—H16A···Se5vii | 0.91 (1) | 2.82 (2) | 3.679 (3) | 159 (4) |
N16—H16B···Se1vii | 0.91 (1) | 2.67 (2) | 3.537 (3) | 160 (4) |
N17—H17A···Se3vii | 0.91 (1) | 3.01 (2) | 3.897 (4) | 166 (4) |
N17—H17B···Se7vii | 0.91 (1) | 3.07 (4) | 3.649 (3) | 124 (3) |
N18—H18A···Se6vii | 0.91 (1) | 2.96 (2) | 3.837 (3) | 162 (3) |
N18—H18B···Se2vii | 0.91 (1) | 2.80 (3) | 3.491 (3) | 134 (3) |
N19—H19A···Se5vii | 0.91 (1) | 2.98 (2) | 3.801 (3) | 151 (4) |
N20—H20A···Se7 | 0.89 (5) | 2.98 (5) | 3.841 (4) | 163 (4) |
N21—H21A···Se8xi | 0.91 (1) | 2.98 (3) | 3.729 (3) | 141 (3) |
N21—H21B···Se2vii | 0.91 (1) | 2.91 (2) | 3.763 (3) | 157 (3) |
N22—H22A···Se5 | 0.91 (1) | 2.97 (2) | 3.785 (3) | 150 (4) |
N22—H22B···Se2vii | 0.91 (1) | 3.10 (3) | 3.818 (4) | 138 (3) |
N23—H23B···Se2vii | 0.91 (1) | 2.60 (1) | 3.505 (3) | 173 (4) |
C1—H1C···Se8xi | 0.99 | 3.14 | 3.702 (4) | 118 |
C6—H6A···Se5i | 0.99 | 2.90 | 3.734 (4) | 143 |
C12—H12C···Se6 | 0.99 | 3.05 | 3.838 (4) | 137 |
C13—H13D···Se8ix | 0.99 | 3.07 | 3.929 (4) | 146 |
N6—H6D···Se4vii | 0.90 (1) | 3.01 (4) | 3.659 (5) | 130 (4) |
C10—H10D···Se8vii | 0.99 | 2.99 | 3.816 (5) | 142 |
N24—H24B···Se3 | 0.91 (1) | 2.77 (5) | 3.327 (4) | 121 (4) |
N24—H24B···Se7 | 0.91 (1) | 2.88 (4) | 3.507 (5) | 128 (4) |
N6A—H6AA···Se4vii | 0.91 | 2.99 | 3.79 (7) | 147 |
C10A—H10F···Se8vii | 0.99 | 2.95 | 3.74 (5) | 137 |
N24A—H24D···Se7 | 0.91 | 3.17 | 3.94 (6) | 145 |
Symmetry codes: (i) −x+1, −y+1, −z+2; (vii) x, y+1, z; (viii) −x+1, −y+1, −z+1; (ix) −x, −y, −z+1; (x) x−1, y+1, z; (xi) x+1, y+1, z. |
Acknowledgements
We thank Daniel Mazur for the preparation of the compound. Core facility BioSupraMol supported by the DFG is acknowledged for X-ray diffraction time.
Funding information
We thank the Verband der Chemischen Industrie e·V. for a Liebig scholarship, and Hans-Böckler-Stiftung for a scholarship for doctoral candidates. The DFG is acknowledged for X-ray diffraction time. We acknowledge support by the Open Access Publication Fund of the Freie Universität Berlin.
References
Blatov, V. A., Shevchenko, A. P. & Proserpio, D. M. (2014). Cryst. Growth Des. 14, 3576–3586. Web of Science CrossRef CAS Google Scholar
Bronger, W., Kimpel, M. & Schmitz, D. (1983). Acta Cryst. B39, 235–238. CrossRef ICSD CAS Web of Science IUCr Journals Google Scholar
Bruker (2016). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Bruker (2021). APEX4. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339–341. Web of Science CrossRef CAS IUCr Journals Google Scholar
Etter, M. C., MacDonald, J. C. & Bernstein, J. (1990). Acta Cryst. B46, 256–262. CrossRef ICSD CAS Web of Science IUCr Journals Google Scholar
Groom, C. R., Bruno, I. J., Lightfoot, M. P. & Ward, S. C. (2016). Acta Cryst. B72, 171–179. Web of Science CrossRef IUCr Journals Google Scholar
Kern, A., Näther, C., Studt, F. & Tuczek, F. (2004). Inorg. Chem. 43, 5003–5010. Web of Science CSD CrossRef PubMed CAS Google Scholar
Kornienko, A., Huebner, L., Freedman, D., Emge, T. J. & Brennan, J. G. (2003). Inorg. Chem. 42, 8476–8480. Web of Science CSD CrossRef PubMed CAS Google Scholar
Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3–10. Web of Science CSD CrossRef ICSD CAS IUCr Journals Google Scholar
Schwarz, M. & Röhr, C. (2015). Inorg. Chem. 54, 1038–1048. Web of Science CrossRef ICSD CAS PubMed Google Scholar
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Stüble, P., Berroth, A. & Röhr, C. (2016). Z. Naturforsch. B, 71, 485–501. Google Scholar
Stüble, P., Peschke, S., Johrendt, D. & Röhr, C. (2018). J. Solid State Chem. 258, 416–430. Google Scholar
Stüble, P. & Röhr, C. (2017). Z. Anorg. Allge Chem. 643, 1462–1473. Google Scholar
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