research communications
Structural characterization of three hydride-bridged sodium aluminate compounds
aWestchem, Department of Pure & Applied Chemistry, University of Strathclyde, 295 Cathedral Street, Glasgow G1 1XL, Scotland, United Kingdom
*Correspondence e-mail: r.e.mulvey@strath.ac.uk
The synthesis and single-crystal structures of three hydride-bridged sodium aluminate compounds containing the utility amide HMDS [N(SiMe3)2 or C6H18NSi2] are reported. Both bis[bis(trimethylsilyl)amido-2κN]-μ-hydrido-hydrido-2κH-(N,N,N′,N′′,N′′-pentamethyldiethylenetriamine-1κ3N,N′,N′′)(tetrahydrofuran-1κO)aluminiumsodium, [AlNa(C6H18NSi2)2H2(C4H8O)(C9H23N3)] or (HMDS)2Al(H)2Na(THF)(PMDETA), (1) (THF = tetrahydrofuran, C4H8O; PMDETA = N,N,N′,N′′,N′′-pentamethyldiethylenetriamine, C9H23N3) and tetrakis[bis(trimethylsilyl)amido]-3κ2N,4κ2N-tetra-μ-hydrido-tetrakis(tetrahydrofuran)-1κ2O,2κ2O-dialuminiumdisodium, [Al2Na2(C6H18NSi2)4H4(C4H8O)4] or [(HMDS)2Al(H)2Na(THF)2]2 (2), are dihydrides. However, 1 is a dinuclear Al—H—Na monomer with one bridging and one terminal hydride ligand whilst in 2 all the hydride ligands bridge between Al and Na atoms to give a dimeric structure with a core (AlHNaH)2 eight-membered ring. In contrast, the structure of bis[bis(trimethylsilyl)amido]-3κN,4κN-dihydrido-3κH,4κH-tetra-μ-hydrido-bis(N,N,N′,N′′,N′′-pentamethyldiethylenetriamine)-1κ3N,N′,N′′;2κ3N,N′,N′′-dialuminiumdisodium, [Al2Na2(C6H18NSi2)2H6(C9H23N3)2] or [(HMDS)Al(H)3Na(PMDETA)]2 (3), also contains a (AlHNaH)2 eight-membered ring but is a trihydride with two bridging and one terminal hydride ligand per Al centre. The (AlHNaH)2 eight-membered rings of 2 and 3 differ in their structural details. That of 2 is based around a twofold axis and has a larger Al⋯Al intra-ring distance than that found in centrosymmetric 3.
1. Chemical context
This work merges two topical areas of chemistry, namely sodium organometallic chemistry and molecular main-group hydride chemistry. Though relatively underdeveloped down the years, the former is currently receiving increased attention driven by the fact that sodium is much more earth-abundant and therefore more sustainable than lithium, an aspect exacerbated by lithium's rapidly escalating usage in battery technology (Yoshio et al., 2009; Lu et al., 2013; Wang et al., 2015; Zhang, 2006). Recent progress has been reported in the use of sodium in cross-coupling catalysis in organic synthesis (Asako et al., 2019) and in the reaction and solvation chemistry of sodium organoamides (Woltornist & Collum, 2021; Ma et al., 2021). As evidenced by a recent 181 page review with the vast majority of studies covered appearing in this century, the latter chemistry is unquestionably a topic of great current interest (Roy et al., 2021; Aldridge & Downs, 2001). Turning to molecular main-group hydrides, compounds have been developed that can mediate a myriad of catalytic reactions that previously were considered the preserve of transition-metal catalysts (Dando et al., 1993; Liptrot et al., 2015; Höllerhage et al., 2021; Spielmann & Harder, 2007; Uhl, 2008).
This study focuses on sodium hydridoaluminates. Though less well known than its lithium congener (LiAlH4), the parent sodium compound in this class, sodium aluminium hydride (NaAlH4) has found use as a reductant or metallating agent (Zakharkin & Gavrilenko, 1962; Walker, 1976; Gavrilenko et al., 1987; Eisler & Chivers, 2006), and has been considered for hydrogen-storage applications (Bogdanović et al., 2000; Sheppard et al., 2013; Fan et al., 2009; Bogdanović et al., 2007). Since our group has enjoyed success in synthesising lithium amido-hydridoaluminates that exhibit bimetallic cooperativity in performing catalytic hydroboration and metallation applications (Pollard et al., 2018), here we set out to synthesize and crystallographically characterize a series of related sodium amido–hydridoaluminates. The structures obtained with just a single amide in the presence of THF and PMDETA are surprisingly diverse.
2. Structural commentary
As shown in Fig. 1, aluminate 1 exists as a hydride-bridged monomer with the four-coordinate aluminium centre in a slightly distorted tetrahedral geometry [bond-angle range 106.2 (15) to 115.12 (10)°; Table 1] and with the geometry of the five-coordinate sodium centre sitting near the centre of the continuum between trigonal–bipyramidal and square-pyrimidal geometries (as shown by a τ5 value of 0.527 using the method of Addison et al., 1984). Bond lengths and angles are given in Table 1. Here the dihydride R2AlH2 unit consists of one terminal hydride ligand and one hydride ligand that bridges between Al and Na.
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Aluminate 2 is also an R2AlH2 dihydride, but here both hydride ligands bridge between Al and Na centres to give the dimer shown in Fig. 2. The core feature is the eight-membered (AlHNaH)2 ring highlighted in Fig. 3. This has crystallographically imposed twofold symmetry, with the 2 axis passing through both the Na1 and Na2 sites. The aluminium centre and both sodium centres occupy 4-coordinate sites with distorted tetrahedral geometries, with the sodium centres much more distorted than the aluminium [range of bond angles = 101.6 (18) to 118.28 (11)° for Al1 and 89.9 (8) to 139.9 (8) and 91.72 (13) to 121.3 (2)° for Na1 and Na2, respectively; Table 2]. Selected geometric parameters are given in Table 2.
Finally, the hydrido-rich RAlH3 aluminate trihydride 3 also exists as a hydride-bridged dimer with the same skeleton of an eight-membered (AlHNaH)2 ring as seen for 2, see Figs. 4 and 5. Structure 3 thus features two bridging hydride ligands and one terminal hydride ligand per Al centre, see Table 3 for selected geometric parameters. Differences between the (AlHNaH)2 rings of compounds 2 and 3 are that the ring of 3 is crystallographically centrosymmetric rather than having the twofold symmetry of 2, and that the Al—H—Na angles of 2 are much closer to linear than the more bent angles found in 3 (compare 154.3 and 163.5° with 109.6 and 132.1°). The near linear and bent geometries result in very different Al⋯Al separation distances for the two compounds [compare 5.6436 (15) and 4.7666 (9) Å for 2 and 3, respectively]. This greater distance is presumably related to the Al centres of 2 each bearing two bulky HMDS ligands whilst the Al centres of 3 each bear only one HMDS ligand. As with 1 and 2, aluminate 3 also contains a four-coordinate, distorted tetrahedral aluminium centre [bond angle range = 102.9 (12)–115.9 (8)°]. Like 1, 3 also features a five-coordinate sodium centre, but here the geometry is closer to square-pyramidal as shown by a τ5 value of 0.077. It is worth noting that Stalke previously reported an Li compound that is analogous with 3. This contained the equivalent eight-membered ring but had two molecules of diethyl ether solvating each lithium centre rather than the chelated PMDETA found here on Na (Heine & Stalke, 1992).
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For 1, the bridging Al1—H1 bond may initially appear to be slightly longer than the terminal Al1—H2 bond [1.59 (3) and 1.54 (3) Å, respectively]. However, the large s.u. values and the general lack of accuracy of H atom positions derived from X-ray data should be kept in mind. Additionally, 3 does not show the expected difference in bridging versus terminal bond lengths, with all Al—H distances essentially equivalent [1.57 (3) Å for the terminal ligand and 1.59 (2) and 1.58 (2) Å for the bridging ligands], whilst the bridging hydrides of 2 are just as short as the terminal bond of 1 [1.53 (3) and 1.55 (3) Å]. Thus there is no reliable experimental evidence herein to support the notion that the bridging Al-hydride bonds should be longer than the terminal ones. All the Na—H bonds in the three compounds are bridging: they have a bond length range from 2.19 (3) Å in 1 to 2.25 (2) Å in 3.
3. Supramolecular features
There are no intermolecular interactions significantly shorter than the sum of van der Waals radii. In all three compounds, the closest contacts are H⋯H contacts between methyl groups or between methyl and CH2 groups. None of the hydride ligands show any significant intermolecular contacts, thus the monomer of 1 and the dimers of 2 and 3 can be described as discrete.
4. Database survey
A search of the Cambridge Structural Database (CSD version 2021.3, update of December 2021; Groom et al., 2016) for [NaXAlX′]2 eight-membered rings similar to that of structures 2 and 3, returned eleven hits; six of these had oxygen as the bridging atom (Muñoz et al., 2014; Wu et al., 2010; Huang et al., 2009; Veith et al., 2008; Nöth et al., 2001), two had nitrogen (Eisler & Chivers, 2006; Böttcher et al., 2001), one had fluorine (Hatop et al., 2000), one had a mix of carbon and oxygen (Huang et al., 2009) and the last hit had a mixture of nitrogen and carbon (Cortes-Llamas & Muñoz-Hernández, 2007).
Searching the CSD for the `Na—H—Al' bridging unit returned just nine hits, with two of these results being NaAlH4 with 15-crown-5 solvating the sodium atom (Sirsch et al., 2010; Olbrich & Trzaska, 2005). This small number of structural precedents showcases the relative novelty of the newly reported structures. The Al—H bonds in these existing compounds have an average length of 1.54 Å for the terminal bonds and 1.57 Å for the bridging interactions; the Na—H bonds are all bridging and have an average length of 2.32 Å. This demonstrates that our results are generally in good agreement with those already reported in literature, although we note that the Na—H bonds reported herein are slightly shorter than the literature average.
There are 87 hits returned in the CSD when a search is carried out for the `Na—HMDS' fragment; this reduces to 78 when only heterobimetallic compounds are considered and reduces to just two hits when `H—Na—HMDS' is searched with one structure being a titanium-hydride compound (Stennett & Power, 2021), and the other a sodium-hydrido magnesiate (Liptrot et al., 2014). When the CSD is searched for `Al—HMDS' it returns 78 results; when only heterobimetallic species are considered this reduces to 46 hits (with 10 of these involving alkali metals) and 29 hits are returned when the `H—Al—HMDS' fragment is searched. These relatively high numbers emphasise the importance of HMDS as a utility ligand in main-group chemistry (Mulvey & Robertson, 2013; Westerhausen, 1998).
5. Synthesis and crystallization
The synthesis of these new sodium aluminium hydride compounds was carried out by metallation via reaction of NaAlH4 with the amine 1,1,1,3,3,3-hexamethyldisilazane in a 1:2 stoichiometric ratio in THF (tetrahydrofuran) solution. After three hours at 313 K, the reaction mixture was left at room temperature for 24 hours. Filtration of the grey suspension that formed resulted in a clear, homogeneous solution. Removal of the solvent in vacuo followed by re-suspension of the residue in hexane, then introduction of a stoichiometric quantity of the donor ligand PMDETA (N,N,N′,N′′,N′′-pentamethyldiethylenetriamine), or THF, resulted in the formation of crystals suitable for single-crystal X-ray This analysis established their identities as the dihydrides (HMDS)2Al(H)(H)Na·(THF)(PMDETA), (1), and [{(HMDS)2Al(H)(H)Na·(THF)2}2], (2), respectively. Attempting to repeat the synthesis of 1, but reducing the room-temperature period from 24hours to 1 hour resulted in the formation of a trihydride product [(HMDS)Al(H)(H)Na·PMDETA]2, (3). The three crystalline products were obtained in yields of 56, 57 and 61%, respectively.
Compound 1: 1H NMR (400.03 MHz, d8-toluene, 300 K): δ 0.48 (s, 36H, CH3 of HMDS); 1.45 (m, J = 3.30 Hz, 8H, CH2 of THF); 1.72 (s, 8H, CH2 of PMDETA); 1.86 (s, 3H, CH3 of PMDETA); 1.94 (s, 12H, CH3 of PMDETA); 3.54 (m, J = 2.25 Hz, 8H, CH2 of THF) ppm. 27Al NMR (104.23 MHz, d8-toluene, 300 K): δ 105.0 (t, J = 164.24) ppm. 13C{1H} NMR (100.59 MHz, d8-toluene, 300 K): δ 6.3 (s, CH3 of HMDS); 25.8 (s, CH2 of THF); 43.6 (s, CH3 of PMDETA); 45.4 (s, CH3 of PMDETA); 54.2 (s, CH2 of PMDETA); 57.0 (s, CH2 of PMDETA); 67.8 (s, CH2 of THF) ppm.
Compound 2: 1H NMR (400.03 MHz, C6D6, 300 K): δ 0.49 (s, 36H, CH3 of HMDS); 1.38 (m, J = 3.47 Hz, 8H, CH2 of THF); 3.50 (m, J = 2.48 Hz, 8H, CH2 of THF) ppm. 27Al NMR (104.23 MHz, C6D6, 300 K); δ 105.4 (s) ppm. 29Si NMR (79.47 MHz, C6D6, 300 K); δ 300 K): δ −3.1 (s) ppm. 13C{1H} NMR (100.59 MHz, C6D6, 300 K); δ 6.3 (s, CH3 of HMDS); 25.5 (s, CH2 of THF); 68.3 (s, CH2 of THF) ppm.
Compound 3: 1H NMR (400.13 MHz, d8-toluene, 300 K): δ 0.45 (s, 18H, CH3 of HMDS); 1.85 (s, 8H, CH2 of PMDETA); 2.09 (s, 3H, CH3 of PMDETA); 2.10 (s, 12H, CH3 of PMDETA) ppm. 27Al NMR (104.23 MHz, d8-toluene, 300 K): δ 106.9 (q, J = 172.62 Hz) ppm. 13C{1H} NMR (100.59 MHz, d8-toluene, 300 K): δ 5.5 (s, CH3 of HMDS); 43.4 (s, CH3 of PMDETA); 45.4 (s, CH3 of PMDETA); 54.8 (s, CH2 of PMDETA); 57.1 (s, CH2 of PMDETA) ppm.
6. details
Crystal data, data collection and structure . For all structures, H atoms bound to C atoms were placed in the expected geometric positions and treated in riding modes. For CH3 groups, C—H = 0.98 Å with Uiso(H) = 1.25Ueq(C) and for CH2 groups, C—H = 0.99 Å with Uiso(H) = 1.2Ueq(C). All hydride H atoms were refined freely and isotropically.
details are summarized in Table 4
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The chosen crystal for structure 2 was treated as a two-component twin and was refined against a hklf 5 formatted reflection file. The twin matrix used was (0 −0.989 0.046 / 0 0.497 0.989 / −1 −0.004 −0.016) and the relative contributions for the twin components refined to 0.841 (4):0.159 (4).
Supporting information
https://doi.org/10.1107/S2056989022010738/hb8043sup1.cif
contains datablocks 1, 2, 3, global. DOI:Structure factors: contains datablock 1. DOI: https://doi.org/10.1107/S2056989022010738/hb80431sup2.hkl
Structure factors: contains datablock 2. DOI: https://doi.org/10.1107/S2056989022010738/hb80432sup3.hkl
Structure factors: contains datablock 3. DOI: https://doi.org/10.1107/S2056989022010738/hb80433sup4.hkl
For all structures, data collection: CrysAlis PRO (Rigaku OD, 2021); cell
CrysAlis PRO (Rigaku OD, 2021); data reduction: CrysAlis PRO (Rigaku OD, 2021). Program(s) used to solve structure: SHELXT (Sheldrick, 2015a) for (1), (2); SHELXS (Sheldrick, 2008) for (3). For all structures, program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: Mercury (Macrae et al., 2020); software used to prepare material for publication: SHELXL (Sheldrick, 2015b).[AlNa(C6H18NSi2)2H2(C4H8O)(C9H23N3)] | F(000) = 1368 |
Mr = 618.18 | Dx = 1.033 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 11.9127 (9) Å | Cell parameters from 5988 reflections |
b = 18.1837 (12) Å | θ = 3.6–26.2° |
c = 18.4076 (13) Å | µ = 0.21 mm−1 |
β = 94.420 (7)° | T = 200 K |
V = 3975.5 (5) Å3 | Block, colourless |
Z = 4 | 0.30 × 0.20 × 0.20 mm |
Oxford Diffraction Gemini E diffractometer | 5685 reflections with I > 2σ(I) |
Radiation source: sealed tube | Rint = 0.063 |
ω scans | θmax = 27.0°, θmin = 3.4° |
Absorption correction: multi-scan (CrysalisPro; Rigaku OD, 2021) | h = −14→14 |
Tmin = 0.763, Tmax = 1.000 | k = −21→23 |
29795 measured reflections | l = −23→23 |
8563 independent reflections |
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.058 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.155 | w = 1/[σ2(Fo2) + (0.0595P)2 + 1.3148P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
8563 reflections | Δρmax = 0.28 e Å−3 |
359 parameters | Δρmin = −0.24 e Å−3 |
0 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 | ||
Al1 | 0.63956 (7) | 0.59440 (4) | 0.80712 (4) | 0.0331 (2) | |
Na1 | 0.55685 (8) | 0.72504 (5) | 0.94113 (5) | 0.0348 (2) | |
Si1 | 0.44880 (7) | 0.52445 (5) | 0.70025 (4) | 0.0448 (2) | |
Si2 | 0.60346 (7) | 0.63621 (4) | 0.64509 (4) | 0.0381 (2) | |
Si3 | 0.85525 (7) | 0.50748 (4) | 0.80247 (4) | 0.0397 (2) | |
Si4 | 0.88537 (7) | 0.66751 (5) | 0.82632 (5) | 0.0437 (2) | |
O1 | 0.68222 (18) | 0.67243 (11) | 1.03006 (11) | 0.0518 (5) | |
N1 | 0.56066 (18) | 0.58335 (12) | 0.71501 (11) | 0.0343 (5) | |
N2 | 0.79757 (18) | 0.59425 (11) | 0.80660 (11) | 0.0344 (5) | |
N3 | 0.5768 (2) | 0.85845 (12) | 0.97529 (13) | 0.0423 (6) | |
N4 | 0.3864 (2) | 0.78852 (14) | 0.88184 (12) | 0.0466 (6) | |
N5 | 0.3906 (2) | 0.66856 (13) | 0.99193 (13) | 0.0438 (6) | |
C1 | 0.4592 (4) | 0.4664 (2) | 0.6168 (2) | 0.0799 (12) | |
H1A | 0.453165 | 0.497888 | 0.573465 | 0.120* | |
H1B | 0.397962 | 0.430276 | 0.613477 | 0.120* | |
H1C | 0.531733 | 0.440805 | 0.619912 | 0.120* | |
C2 | 0.4317 (3) | 0.4567 (2) | 0.7748 (2) | 0.0759 (12) | |
H2A | 0.499070 | 0.425762 | 0.781334 | 0.114* | |
H2B | 0.365773 | 0.425688 | 0.762000 | 0.114* | |
H2C | 0.421113 | 0.482991 | 0.820250 | 0.114* | |
C3 | 0.3115 (3) | 0.5748 (3) | 0.6918 (2) | 0.0854 (13) | |
H3A | 0.300833 | 0.600689 | 0.737434 | 0.128* | |
H3B | 0.249910 | 0.539693 | 0.681527 | 0.128* | |
H3C | 0.311754 | 0.610512 | 0.651871 | 0.128* | |
C4 | 0.4936 (3) | 0.6539 (2) | 0.56844 (18) | 0.0660 (10) | |
H4A | 0.472300 | 0.607375 | 0.544316 | 0.099* | |
H4B | 0.523876 | 0.687488 | 0.533180 | 0.099* | |
H4C | 0.427118 | 0.676149 | 0.587811 | 0.099* | |
C5 | 0.7243 (3) | 0.59371 (19) | 0.60198 (18) | 0.0623 (10) | |
H5A | 0.787843 | 0.587871 | 0.638592 | 0.093* | |
H5B | 0.746598 | 0.625467 | 0.562570 | 0.093* | |
H5C | 0.701865 | 0.545431 | 0.582120 | 0.093* | |
C6 | 0.6453 (3) | 0.73071 (16) | 0.67637 (18) | 0.0565 (8) | |
H6A | 0.580992 | 0.755089 | 0.696218 | 0.085* | |
H6B | 0.669284 | 0.759156 | 0.635073 | 0.085* | |
H6C | 0.707629 | 0.727456 | 0.714223 | 0.085* | |
C7 | 0.7618 (3) | 0.44199 (16) | 0.74853 (18) | 0.0561 (8) | |
H7A | 0.689997 | 0.437673 | 0.770779 | 0.084* | |
H7B | 0.798140 | 0.393656 | 0.747910 | 0.084* | |
H7C | 0.748243 | 0.460203 | 0.698514 | 0.084* | |
C8 | 0.9917 (3) | 0.50652 (19) | 0.75711 (18) | 0.0598 (9) | |
H8A | 0.978653 | 0.524917 | 0.707126 | 0.090* | |
H8B | 1.020649 | 0.456114 | 0.756174 | 0.090* | |
H8C | 1.046738 | 0.538037 | 0.784416 | 0.090* | |
C9 | 0.8824 (3) | 0.46502 (17) | 0.89489 (17) | 0.0515 (8) | |
H9A | 0.941049 | 0.493006 | 0.923096 | 0.077* | |
H9B | 0.907408 | 0.414071 | 0.889685 | 0.077* | |
H9C | 0.813040 | 0.465772 | 0.920227 | 0.077* | |
C10 | 0.8152 (3) | 0.74902 (17) | 0.8652 (2) | 0.0608 (9) | |
H10A | 0.750759 | 0.763914 | 0.832232 | 0.091* | |
H10B | 0.869008 | 0.789767 | 0.871064 | 0.091* | |
H10C | 0.789172 | 0.736068 | 0.912808 | 0.091* | |
C11 | 1.0014 (3) | 0.6463 (2) | 0.8979 (2) | 0.0668 (10) | |
H11A | 0.968960 | 0.628249 | 0.941836 | 0.100* | |
H11B | 1.045002 | 0.691043 | 0.909527 | 0.100* | |
H11C | 1.050798 | 0.608593 | 0.879638 | 0.100* | |
C12 | 0.9562 (3) | 0.7009 (2) | 0.7452 (2) | 0.0727 (11) | |
H12A | 1.007383 | 0.662841 | 0.729602 | 0.109* | |
H12B | 0.998983 | 0.745648 | 0.758126 | 0.109* | |
H12C | 0.899180 | 0.711685 | 0.705338 | 0.109* | |
C13 | 0.7129 (4) | 0.59808 (19) | 1.0185 (2) | 0.0794 (13) | |
H13A | 0.739248 | 0.592384 | 0.969087 | 0.095* | |
H13B | 0.646853 | 0.565664 | 1.022377 | 0.095* | |
C14 | 0.8028 (3) | 0.5774 (2) | 1.0734 (2) | 0.0657 (10) | |
H14A | 0.866077 | 0.553911 | 1.050396 | 0.079* | |
H14B | 0.774472 | 0.543060 | 1.109473 | 0.079* | |
C15 | 0.8383 (4) | 0.6473 (2) | 1.1081 (2) | 0.0865 (14) | |
H15A | 0.903577 | 0.668296 | 1.085061 | 0.104* | |
H15B | 0.859096 | 0.640319 | 1.160768 | 0.104* | |
C16 | 0.7383 (3) | 0.6958 (2) | 1.0963 (2) | 0.0650 (10) | |
H16A | 0.688769 | 0.690686 | 1.136820 | 0.078* | |
H16B | 0.761539 | 0.747928 | 1.093089 | 0.078* | |
C17 | 0.6899 (3) | 0.89006 (19) | 0.9743 (2) | 0.0654 (10) | |
H17A | 0.742078 | 0.862904 | 1.008247 | 0.098* | |
H17B | 0.688110 | 0.941800 | 0.989076 | 0.098* | |
H17C | 0.715079 | 0.886581 | 0.924999 | 0.098* | |
C18 | 0.5413 (3) | 0.86402 (18) | 1.04925 (17) | 0.0578 (9) | |
H18A | 0.467986 | 0.840096 | 1.051605 | 0.087* | |
H18B | 0.535260 | 0.915954 | 1.062622 | 0.087* | |
H18C | 0.596965 | 0.839744 | 1.083183 | 0.087* | |
C19 | 0.5011 (3) | 0.89715 (17) | 0.92279 (18) | 0.0578 (9) | |
H19A | 0.535441 | 0.898517 | 0.875505 | 0.069* | |
H19B | 0.493323 | 0.948554 | 0.939388 | 0.069* | |
C20 | 0.3867 (3) | 0.86384 (18) | 0.91131 (19) | 0.0594 (9) | |
H20A | 0.351778 | 0.863152 | 0.958411 | 0.071* | |
H20B | 0.339517 | 0.895394 | 0.877408 | 0.071* | |
C21 | 0.3929 (3) | 0.7908 (2) | 0.80280 (17) | 0.0719 (11) | |
H21A | 0.459166 | 0.819221 | 0.791375 | 0.108* | |
H21B | 0.324847 | 0.814149 | 0.779988 | 0.108* | |
H21C | 0.398900 | 0.740625 | 0.784108 | 0.108* | |
C22 | 0.2871 (3) | 0.7477 (2) | 0.89959 (19) | 0.0603 (9) | |
H22A | 0.275253 | 0.706168 | 0.865093 | 0.072* | |
H22B | 0.220562 | 0.780358 | 0.892814 | 0.072* | |
C23 | 0.2948 (3) | 0.71804 (19) | 0.97632 (17) | 0.0553 (8) | |
H23A | 0.301165 | 0.759769 | 1.010931 | 0.066* | |
H23B | 0.224432 | 0.691265 | 0.984341 | 0.066* | |
C24 | 0.4038 (3) | 0.6565 (2) | 1.07060 (19) | 0.0701 (10) | |
H24A | 0.469178 | 0.624809 | 1.082520 | 0.105* | |
H24B | 0.336009 | 0.632814 | 1.086492 | 0.105* | |
H24C | 0.415160 | 0.703849 | 1.095551 | 0.105* | |
C25 | 0.3733 (4) | 0.5992 (2) | 0.9539 (2) | 0.0809 (12) | |
H25A | 0.376104 | 0.607081 | 0.901433 | 0.121* | |
H25B | 0.299568 | 0.579044 | 0.963589 | 0.121* | |
H25C | 0.432434 | 0.564443 | 0.971050 | 0.121* | |
H1 | 0.598 (2) | 0.6691 (15) | 0.8409 (15) | 0.052 (8)* | |
H2 | 0.607 (2) | 0.5328 (15) | 0.8589 (15) | 0.052 (8)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.0318 (4) | 0.0404 (5) | 0.0275 (4) | 0.0016 (3) | 0.0042 (3) | −0.0022 (3) |
Na1 | 0.0359 (6) | 0.0337 (6) | 0.0350 (5) | 0.0033 (4) | 0.0037 (4) | −0.0001 (4) |
Si1 | 0.0394 (5) | 0.0590 (5) | 0.0357 (4) | −0.0115 (4) | 0.0002 (4) | 0.0008 (4) |
Si2 | 0.0414 (5) | 0.0422 (5) | 0.0314 (4) | 0.0027 (3) | 0.0065 (3) | 0.0047 (3) |
Si3 | 0.0384 (4) | 0.0408 (4) | 0.0400 (4) | 0.0079 (3) | 0.0036 (3) | −0.0035 (3) |
Si4 | 0.0397 (5) | 0.0446 (5) | 0.0469 (5) | −0.0087 (4) | 0.0047 (4) | −0.0040 (4) |
O1 | 0.0556 (13) | 0.0492 (13) | 0.0482 (12) | 0.0099 (10) | −0.0120 (10) | 0.0016 (10) |
N1 | 0.0322 (12) | 0.0434 (13) | 0.0275 (11) | 0.0004 (10) | 0.0045 (9) | 0.0001 (9) |
N2 | 0.0336 (12) | 0.0350 (12) | 0.0349 (12) | 0.0023 (9) | 0.0032 (10) | −0.0022 (10) |
N3 | 0.0510 (15) | 0.0330 (13) | 0.0439 (13) | 0.0007 (11) | 0.0094 (12) | 0.0015 (10) |
N4 | 0.0460 (15) | 0.0570 (16) | 0.0367 (13) | 0.0075 (12) | 0.0030 (11) | 0.0063 (12) |
N5 | 0.0441 (14) | 0.0431 (14) | 0.0447 (14) | −0.0069 (11) | 0.0059 (11) | 0.0040 (11) |
C1 | 0.101 (3) | 0.083 (3) | 0.055 (2) | −0.034 (2) | 0.007 (2) | −0.023 (2) |
C2 | 0.073 (3) | 0.090 (3) | 0.062 (2) | −0.041 (2) | −0.0040 (19) | 0.017 (2) |
C3 | 0.039 (2) | 0.120 (3) | 0.096 (3) | −0.005 (2) | −0.003 (2) | 0.011 (3) |
C4 | 0.075 (3) | 0.074 (2) | 0.0466 (19) | 0.0054 (19) | −0.0068 (18) | 0.0160 (17) |
C5 | 0.072 (2) | 0.064 (2) | 0.055 (2) | 0.0109 (18) | 0.0310 (18) | 0.0117 (17) |
C6 | 0.073 (2) | 0.0442 (18) | 0.0532 (19) | −0.0041 (16) | 0.0105 (17) | 0.0077 (15) |
C7 | 0.070 (2) | 0.0357 (17) | 0.061 (2) | 0.0084 (15) | −0.0011 (17) | −0.0102 (15) |
C8 | 0.051 (2) | 0.070 (2) | 0.061 (2) | 0.0158 (17) | 0.0163 (17) | −0.0086 (17) |
C9 | 0.0486 (19) | 0.0513 (19) | 0.0542 (19) | 0.0080 (14) | 0.0006 (15) | 0.0055 (15) |
C10 | 0.067 (2) | 0.0426 (18) | 0.072 (2) | −0.0112 (16) | 0.0024 (19) | −0.0153 (16) |
C11 | 0.050 (2) | 0.076 (2) | 0.072 (2) | −0.0141 (17) | −0.0112 (18) | −0.011 (2) |
C12 | 0.069 (2) | 0.079 (3) | 0.073 (2) | −0.020 (2) | 0.019 (2) | 0.010 (2) |
C13 | 0.095 (3) | 0.052 (2) | 0.084 (3) | 0.0189 (19) | −0.041 (2) | −0.018 (2) |
C14 | 0.063 (2) | 0.067 (2) | 0.065 (2) | 0.0156 (18) | −0.0102 (19) | −0.0038 (19) |
C15 | 0.080 (3) | 0.081 (3) | 0.091 (3) | 0.026 (2) | −0.043 (2) | −0.029 (2) |
C16 | 0.065 (2) | 0.058 (2) | 0.068 (2) | 0.0061 (17) | −0.0147 (19) | −0.0146 (18) |
C17 | 0.068 (2) | 0.057 (2) | 0.073 (2) | −0.0197 (18) | 0.016 (2) | −0.0072 (18) |
C18 | 0.078 (2) | 0.0506 (19) | 0.0462 (18) | 0.0016 (17) | 0.0128 (17) | −0.0060 (15) |
C19 | 0.079 (3) | 0.0402 (18) | 0.0543 (19) | 0.0095 (17) | 0.0064 (18) | 0.0056 (15) |
C20 | 0.061 (2) | 0.055 (2) | 0.062 (2) | 0.0246 (17) | 0.0062 (18) | 0.0155 (17) |
C21 | 0.082 (3) | 0.092 (3) | 0.0418 (18) | 0.011 (2) | 0.0010 (18) | 0.0126 (19) |
C22 | 0.0409 (18) | 0.077 (2) | 0.062 (2) | 0.0038 (16) | −0.0059 (16) | 0.0061 (18) |
C23 | 0.0389 (18) | 0.071 (2) | 0.0568 (19) | −0.0030 (16) | 0.0111 (15) | 0.0008 (17) |
C24 | 0.071 (2) | 0.084 (3) | 0.056 (2) | −0.017 (2) | 0.0095 (18) | 0.0195 (19) |
C25 | 0.087 (3) | 0.059 (2) | 0.099 (3) | −0.016 (2) | 0.026 (3) | −0.014 (2) |
Al1—N2 | 1.883 (2) | C7—H7A | 0.9800 |
Al1—N1 | 1.885 (2) | C7—H7B | 0.9800 |
Al1—H1 | 1.59 (3) | C7—H7C | 0.9800 |
Al1—H2 | 1.54 (3) | C8—H8A | 0.9800 |
Na1—O1 | 2.334 (2) | C8—H8B | 0.9800 |
Na1—N5 | 2.477 (3) | C8—H8C | 0.9800 |
Na1—N4 | 2.511 (3) | C9—H9A | 0.9800 |
Na1—N3 | 2.513 (2) | C9—H9B | 0.9800 |
Na1—H1 | 2.19 (3) | C9—H9C | 0.9800 |
Si1—N1 | 1.715 (2) | C10—H10A | 0.9800 |
Si1—C2 | 1.868 (3) | C10—H10B | 0.9800 |
Si1—C3 | 1.871 (4) | C10—H10C | 0.9800 |
Si1—C1 | 1.875 (4) | C11—H11A | 0.9800 |
Si2—N1 | 1.715 (2) | C11—H11B | 0.9800 |
Si2—C5 | 1.864 (3) | C11—H11C | 0.9800 |
Si2—C6 | 1.868 (3) | C12—H12A | 0.9800 |
Si2—C4 | 1.877 (3) | C12—H12B | 0.9800 |
Si3—N2 | 1.725 (2) | C12—H12C | 0.9800 |
Si3—C7 | 1.863 (3) | C13—C14 | 1.464 (5) |
Si3—C9 | 1.873 (3) | C13—H13A | 0.9900 |
Si3—C8 | 1.884 (3) | C13—H13B | 0.9900 |
Si4—N2 | 1.715 (2) | C14—C15 | 1.470 (5) |
Si4—C10 | 1.871 (3) | C14—H14A | 0.9900 |
Si4—C12 | 1.872 (3) | C14—H14B | 0.9900 |
Si4—C11 | 1.874 (4) | C15—C16 | 1.485 (5) |
O1—C16 | 1.411 (4) | C15—H15A | 0.9900 |
O1—C13 | 1.421 (4) | C15—H15B | 0.9900 |
N3—C19 | 1.451 (4) | C16—H16A | 0.9900 |
N3—C18 | 1.460 (4) | C16—H16B | 0.9900 |
N3—C17 | 1.466 (4) | C17—H17A | 0.9800 |
N4—C22 | 1.455 (4) | C17—H17B | 0.9800 |
N4—C21 | 1.463 (4) | C17—H17C | 0.9800 |
N4—C20 | 1.473 (4) | C18—H18A | 0.9800 |
N5—C25 | 1.450 (4) | C18—H18B | 0.9800 |
N5—C24 | 1.461 (4) | C18—H18C | 0.9800 |
N5—C23 | 1.464 (4) | C19—C20 | 1.492 (5) |
C1—H1A | 0.9800 | C19—H19A | 0.9900 |
C1—H1B | 0.9800 | C19—H19B | 0.9900 |
C1—H1C | 0.9800 | C20—H20A | 0.9900 |
C2—H2A | 0.9800 | C20—H20B | 0.9900 |
C2—H2B | 0.9800 | C21—H21A | 0.9800 |
C2—H2C | 0.9800 | C21—H21B | 0.9800 |
C3—H3A | 0.9800 | C21—H21C | 0.9800 |
C3—H3B | 0.9800 | C22—C23 | 1.508 (4) |
C3—H3C | 0.9800 | C22—H22A | 0.9900 |
C4—H4A | 0.9800 | C22—H22B | 0.9900 |
C4—H4B | 0.9800 | C23—H23A | 0.9900 |
C4—H4C | 0.9800 | C23—H23B | 0.9900 |
C5—H5A | 0.9800 | C24—H24A | 0.9800 |
C5—H5B | 0.9800 | C24—H24B | 0.9800 |
C5—H5C | 0.9800 | C24—H24C | 0.9800 |
C6—H6A | 0.9800 | C25—H25A | 0.9800 |
C6—H6B | 0.9800 | C25—H25B | 0.9800 |
C6—H6C | 0.9800 | C25—H25C | 0.9800 |
N2—Al1—N1 | 115.12 (10) | Si3—C8—H8A | 109.5 |
N2—Al1—H1 | 110.3 (11) | Si3—C8—H8B | 109.5 |
N1—Al1—H1 | 107.0 (10) | H8A—C8—H8B | 109.5 |
N2—Al1—H2 | 107.5 (11) | Si3—C8—H8C | 109.5 |
N1—Al1—H2 | 110.4 (11) | H8A—C8—H8C | 109.5 |
H1—Al1—H2 | 106.2 (15) | H8B—C8—H8C | 109.5 |
O1—Na1—N5 | 93.00 (9) | Si3—C9—H9A | 109.5 |
O1—Na1—N4 | 161.00 (9) | Si3—C9—H9B | 109.5 |
N5—Na1—N4 | 73.23 (9) | H9A—C9—H9B | 109.5 |
O1—Na1—N3 | 100.21 (8) | Si3—C9—H9C | 109.5 |
N5—Na1—N3 | 111.63 (9) | H9A—C9—H9C | 109.5 |
N4—Na1—N3 | 73.89 (9) | H9B—C9—H9C | 109.5 |
O1—Na1—H1 | 103.2 (7) | Si4—C10—H10A | 109.5 |
N5—Na1—H1 | 111.1 (8) | Si4—C10—H10B | 109.5 |
N4—Na1—H1 | 94.1 (8) | H10A—C10—H10B | 109.5 |
N3—Na1—H1 | 129.4 (7) | Si4—C10—H10C | 109.5 |
N1—Si1—C2 | 115.05 (14) | H10A—C10—H10C | 109.5 |
N1—Si1—C3 | 111.78 (16) | H10B—C10—H10C | 109.5 |
C2—Si1—C3 | 103.9 (2) | Si4—C11—H11A | 109.5 |
N1—Si1—C1 | 112.45 (15) | Si4—C11—H11B | 109.5 |
C2—Si1—C1 | 104.39 (19) | H11A—C11—H11B | 109.5 |
C3—Si1—C1 | 108.6 (2) | Si4—C11—H11C | 109.5 |
N1—Si2—C5 | 111.77 (13) | H11A—C11—H11C | 109.5 |
N1—Si2—C6 | 111.84 (12) | H11B—C11—H11C | 109.5 |
C5—Si2—C6 | 108.43 (16) | Si4—C12—H12A | 109.5 |
N1—Si2—C4 | 115.45 (14) | Si4—C12—H12B | 109.5 |
C5—Si2—C4 | 105.54 (17) | H12A—C12—H12B | 109.5 |
C6—Si2—C4 | 103.18 (17) | Si4—C12—H12C | 109.5 |
N2—Si3—C7 | 112.61 (13) | H12A—C12—H12C | 109.5 |
N2—Si3—C9 | 112.24 (12) | H12B—C12—H12C | 109.5 |
C7—Si3—C9 | 105.96 (15) | O1—C13—C14 | 108.9 (3) |
N2—Si3—C8 | 112.84 (13) | O1—C13—H13A | 109.9 |
C7—Si3—C8 | 104.96 (15) | C14—C13—H13A | 109.9 |
C9—Si3—C8 | 107.70 (15) | O1—C13—H13B | 109.9 |
N2—Si4—C10 | 114.41 (13) | C14—C13—H13B | 109.9 |
N2—Si4—C12 | 112.82 (15) | H13A—C13—H13B | 108.3 |
C10—Si4—C12 | 106.89 (17) | C13—C14—C15 | 104.5 (3) |
N2—Si4—C11 | 113.19 (14) | C13—C14—H14A | 110.9 |
C10—Si4—C11 | 102.75 (17) | C15—C14—H14A | 110.9 |
C12—Si4—C11 | 105.92 (18) | C13—C14—H14B | 110.9 |
C16—O1—C13 | 107.9 (2) | C15—C14—H14B | 110.9 |
C16—O1—Na1 | 135.86 (19) | H14A—C14—H14B | 108.9 |
C13—O1—Na1 | 116.29 (19) | C14—C15—C16 | 104.4 (3) |
Si1—N1—Si2 | 120.23 (13) | C14—C15—H15A | 110.9 |
Si1—N1—Al1 | 122.45 (12) | C16—C15—H15A | 110.9 |
Si2—N1—Al1 | 117.31 (12) | C14—C15—H15B | 110.9 |
Si4—N2—Si3 | 118.77 (13) | C16—C15—H15B | 110.9 |
Si4—N2—Al1 | 126.25 (12) | H15A—C15—H15B | 108.9 |
Si3—N2—Al1 | 113.78 (12) | O1—C16—C15 | 105.6 (3) |
C19—N3—C18 | 112.2 (3) | O1—C16—H16A | 110.6 |
C19—N3—C17 | 109.0 (3) | C15—C16—H16A | 110.6 |
C18—N3—C17 | 108.4 (3) | O1—C16—H16B | 110.6 |
C19—N3—Na1 | 105.05 (18) | C15—C16—H16B | 110.6 |
C18—N3—Na1 | 105.78 (17) | H16A—C16—H16B | 108.8 |
C17—N3—Na1 | 116.38 (19) | N3—C17—H17A | 109.5 |
C22—N4—C21 | 110.1 (3) | N3—C17—H17B | 109.5 |
C22—N4—C20 | 111.7 (3) | H17A—C17—H17B | 109.5 |
C21—N4—C20 | 109.9 (3) | N3—C17—H17C | 109.5 |
C22—N4—Na1 | 108.21 (18) | H17A—C17—H17C | 109.5 |
C21—N4—Na1 | 110.0 (2) | H17B—C17—H17C | 109.5 |
C20—N4—Na1 | 106.78 (18) | N3—C18—H18A | 109.5 |
C25—N5—C24 | 110.4 (3) | N3—C18—H18B | 109.5 |
C25—N5—C23 | 111.1 (3) | H18A—C18—H18B | 109.5 |
C24—N5—C23 | 108.0 (3) | N3—C18—H18C | 109.5 |
C25—N5—Na1 | 105.5 (2) | H18A—C18—H18C | 109.5 |
C24—N5—Na1 | 114.1 (2) | H18B—C18—H18C | 109.5 |
C23—N5—Na1 | 107.76 (17) | N3—C19—C20 | 114.3 (3) |
Si1—C1—H1A | 109.5 | N3—C19—H19A | 108.7 |
Si1—C1—H1B | 109.5 | C20—C19—H19A | 108.7 |
H1A—C1—H1B | 109.5 | N3—C19—H19B | 108.7 |
Si1—C1—H1C | 109.5 | C20—C19—H19B | 108.7 |
H1A—C1—H1C | 109.5 | H19A—C19—H19B | 107.6 |
H1B—C1—H1C | 109.5 | N4—C20—C19 | 113.9 (3) |
Si1—C2—H2A | 109.5 | N4—C20—H20A | 108.8 |
Si1—C2—H2B | 109.5 | C19—C20—H20A | 108.8 |
H2A—C2—H2B | 109.5 | N4—C20—H20B | 108.8 |
Si1—C2—H2C | 109.5 | C19—C20—H20B | 108.8 |
H2A—C2—H2C | 109.5 | H20A—C20—H20B | 107.7 |
H2B—C2—H2C | 109.5 | N4—C21—H21A | 109.5 |
Si1—C3—H3A | 109.5 | N4—C21—H21B | 109.5 |
Si1—C3—H3B | 109.5 | H21A—C21—H21B | 109.5 |
H3A—C3—H3B | 109.5 | N4—C21—H21C | 109.5 |
Si1—C3—H3C | 109.5 | H21A—C21—H21C | 109.5 |
H3A—C3—H3C | 109.5 | H21B—C21—H21C | 109.5 |
H3B—C3—H3C | 109.5 | N4—C22—C23 | 113.6 (3) |
Si2—C4—H4A | 109.5 | N4—C22—H22A | 108.8 |
Si2—C4—H4B | 109.5 | C23—C22—H22A | 108.8 |
H4A—C4—H4B | 109.5 | N4—C22—H22B | 108.8 |
Si2—C4—H4C | 109.5 | C23—C22—H22B | 108.8 |
H4A—C4—H4C | 109.5 | H22A—C22—H22B | 107.7 |
H4B—C4—H4C | 109.5 | N5—C23—C22 | 113.2 (3) |
Si2—C5—H5A | 109.5 | N5—C23—H23A | 108.9 |
Si2—C5—H5B | 109.5 | C22—C23—H23A | 108.9 |
H5A—C5—H5B | 109.5 | N5—C23—H23B | 108.9 |
Si2—C5—H5C | 109.5 | C22—C23—H23B | 108.9 |
H5A—C5—H5C | 109.5 | H23A—C23—H23B | 107.8 |
H5B—C5—H5C | 109.5 | N5—C24—H24A | 109.5 |
Si2—C6—H6A | 109.5 | N5—C24—H24B | 109.5 |
Si2—C6—H6B | 109.5 | H24A—C24—H24B | 109.5 |
H6A—C6—H6B | 109.5 | N5—C24—H24C | 109.5 |
Si2—C6—H6C | 109.5 | H24A—C24—H24C | 109.5 |
H6A—C6—H6C | 109.5 | H24B—C24—H24C | 109.5 |
H6B—C6—H6C | 109.5 | N5—C25—H25A | 109.5 |
Si3—C7—H7A | 109.5 | N5—C25—H25B | 109.5 |
Si3—C7—H7B | 109.5 | H25A—C25—H25B | 109.5 |
H7A—C7—H7B | 109.5 | N5—C25—H25C | 109.5 |
Si3—C7—H7C | 109.5 | H25A—C25—H25C | 109.5 |
H7A—C7—H7C | 109.5 | H25B—C25—H25C | 109.5 |
H7B—C7—H7C | 109.5 | ||
C2—Si1—N1—Si2 | 167.40 (19) | C8—Si3—N2—Al1 | 151.73 (15) |
C3—Si1—N1—Si2 | −74.4 (2) | N1—Al1—N2—Si4 | 112.19 (15) |
C1—Si1—N1—Si2 | 48.1 (2) | N1—Al1—N2—Si3 | −80.58 (14) |
C2—Si1—N1—Al1 | −13.7 (2) | C16—O1—C13—C14 | −8.2 (5) |
C3—Si1—N1—Al1 | 104.5 (2) | Na1—O1—C13—C14 | 172.3 (3) |
C1—Si1—N1—Al1 | −133.02 (19) | O1—C13—C14—C15 | −11.0 (5) |
C5—Si2—N1—Si1 | −97.36 (19) | C13—C14—C15—C16 | 24.8 (5) |
C6—Si2—N1—Si1 | 140.84 (16) | C13—O1—C16—C15 | 23.9 (4) |
C4—Si2—N1—Si1 | 23.3 (2) | Na1—O1—C16—C15 | −156.7 (3) |
C5—Si2—N1—Al1 | 83.68 (18) | C14—C15—C16—O1 | −30.4 (5) |
C6—Si2—N1—Al1 | −38.12 (19) | C18—N3—C19—C20 | −67.6 (4) |
C4—Si2—N1—Al1 | −155.69 (16) | C17—N3—C19—C20 | 172.3 (3) |
N2—Al1—N1—Si1 | 134.48 (13) | Na1—N3—C19—C20 | 46.9 (3) |
N2—Al1—N1—Si2 | −46.58 (16) | C22—N4—C20—C19 | 155.9 (3) |
C10—Si4—N2—Si3 | −156.81 (16) | C21—N4—C20—C19 | −81.5 (3) |
C12—Si4—N2—Si3 | 80.7 (2) | Na1—N4—C20—C19 | 37.8 (3) |
C11—Si4—N2—Si3 | −39.6 (2) | N3—C19—C20—N4 | −62.2 (4) |
C10—Si4—N2—Al1 | 9.8 (2) | C21—N4—C22—C23 | 158.3 (3) |
C12—Si4—N2—Al1 | −112.65 (19) | C20—N4—C22—C23 | −79.3 (3) |
C11—Si4—N2—Al1 | 127.09 (18) | Na1—N4—C22—C23 | 38.0 (3) |
C7—Si3—N2—Si4 | −158.62 (15) | C25—N5—C23—C22 | −71.0 (4) |
C9—Si3—N2—Si4 | 81.91 (17) | C24—N5—C23—C22 | 167.7 (3) |
C8—Si3—N2—Si4 | −40.01 (19) | Na1—N5—C23—C22 | 44.0 (3) |
C7—Si3—N2—Al1 | 33.12 (18) | N4—C22—C23—N5 | −58.8 (4) |
C9—Si3—N2—Al1 | −86.35 (16) |
[Al2Na2(C6H18NSi2)4H4(C4H8O)4] | F(000) = 2272 |
Mr = 1033.96 | Dx = 1.088 Mg m−3 |
Monoclinic, C2/c | Cu Kα radiation, λ = 1.54184 Å |
a = 22.4151 (4) Å | Cell parameters from 24656 reflections |
b = 17.2323 (2) Å | θ = 2.7–72.5° |
c = 17.4649 (3) Å | µ = 2.29 mm−1 |
β = 110.674 (2)° | T = 100 K |
V = 6311.64 (19) Å3 | Fragment, colourless |
Z = 4 | 0.25 × 0.20 × 0.10 mm |
Rigaku Synergy-i diffractometer | 5781 reflections with I > 2σ(I) |
Radiation source: microsource tube | Rint = 0.063 |
ω scans | θmax = 72.8°, θmin = 3.3° |
Absorption correction: multi-scan (CrysalisPro; Rigaku OD, 2021) | h = −27→27 |
Tmin = 0.121, Tmax = 1.000 | k = −21→21 |
40833 measured reflections | l = −21→21 |
6268 independent reflections |
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.053 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.160 | w = 1/[σ2(Fo2) + (0.0641P)2 + 17.678P] where P = (Fo2 + 2Fc2)/3 |
S = 1.13 | (Δ/σ)max = 0.001 |
6268 reflections | Δρmax = 0.36 e Å−3 |
293 parameters | Δρmin = −0.42 e Å−3 |
0 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. |
Refinement. Refined as a two-component twin. |
x | y | z | Uiso*/Ueq | ||
Al1 | 0.48738 (4) | 0.74554 (5) | 0.40514 (5) | 0.02599 (19) | |
Na1 | 0.500000 | 0.88645 (9) | 0.250000 | 0.0325 (4) | |
Na2 | 0.500000 | 0.61172 (9) | 0.250000 | 0.0341 (4) | |
Si1 | 0.62196 (4) | 0.80971 (4) | 0.46633 (5) | 0.02963 (19) | |
Si2 | 0.58845 (4) | 0.68549 (4) | 0.56835 (5) | 0.02967 (19) | |
Si3 | 0.41149 (4) | 0.81457 (4) | 0.50915 (5) | 0.02863 (19) | |
Si4 | 0.34965 (4) | 0.69261 (5) | 0.38716 (5) | 0.0320 (2) | |
O1 | 0.57142 (11) | 0.97423 (12) | 0.23571 (13) | 0.0377 (5) | |
O2 | 0.57085 (12) | 0.52024 (13) | 0.31969 (13) | 0.0460 (6) | |
N1 | 0.56860 (11) | 0.74909 (13) | 0.48689 (14) | 0.0272 (5) | |
N2 | 0.41601 (11) | 0.74821 (13) | 0.43715 (14) | 0.0278 (5) | |
C1 | 0.59865 (16) | 0.91507 (18) | 0.4541 (2) | 0.0385 (7) | |
H1A | 0.554713 | 0.920006 | 0.415707 | 0.058* | |
H1B | 0.627356 | 0.943553 | 0.432883 | 0.058* | |
H1C | 0.601733 | 0.936564 | 0.507309 | 0.058* | |
C2 | 0.70269 (15) | 0.8121 (2) | 0.5490 (2) | 0.0436 (8) | |
H2A | 0.698200 | 0.825640 | 0.601215 | 0.065* | |
H2B | 0.729328 | 0.850928 | 0.535467 | 0.065* | |
H2C | 0.722745 | 0.760917 | 0.553606 | 0.065* | |
C3 | 0.63416 (15) | 0.7790 (2) | 0.36960 (19) | 0.0381 (7) | |
H3A | 0.654264 | 0.727664 | 0.377494 | 0.057* | |
H3B | 0.661732 | 0.816621 | 0.356140 | 0.057* | |
H3C | 0.592847 | 0.776663 | 0.324765 | 0.057* | |
C4 | 0.66680 (16) | 0.63313 (19) | 0.5912 (2) | 0.0436 (8) | |
H4A | 0.676244 | 0.627973 | 0.540759 | 0.065* | |
H4B | 0.663986 | 0.581467 | 0.613140 | 0.065* | |
H4C | 0.700857 | 0.662756 | 0.631567 | 0.065* | |
C5 | 0.59591 (16) | 0.73563 (19) | 0.66691 (18) | 0.0392 (7) | |
H5A | 0.627146 | 0.777728 | 0.677101 | 0.059* | |
H5B | 0.610032 | 0.698241 | 0.712042 | 0.059* | |
H5C | 0.554421 | 0.757047 | 0.662961 | 0.059* | |
C6 | 0.52614 (16) | 0.60790 (18) | 0.54800 (19) | 0.0384 (7) | |
H6A | 0.484882 | 0.631662 | 0.541356 | 0.058* | |
H6B | 0.537915 | 0.571569 | 0.594118 | 0.058* | |
H6C | 0.523034 | 0.579928 | 0.497882 | 0.058* | |
C7 | 0.47767 (14) | 0.88716 (17) | 0.53522 (18) | 0.0330 (6) | |
H7A | 0.518695 | 0.860368 | 0.558584 | 0.050* | |
H7B | 0.472896 | 0.924276 | 0.575190 | 0.050* | |
H7C | 0.476106 | 0.914898 | 0.485563 | 0.050* | |
C8 | 0.33596 (15) | 0.87377 (18) | 0.4736 (2) | 0.0367 (7) | |
H8A | 0.333389 | 0.902770 | 0.424218 | 0.055* | |
H8B | 0.336152 | 0.910169 | 0.516749 | 0.055* | |
H8C | 0.299062 | 0.839154 | 0.461174 | 0.055* | |
C9 | 0.41473 (17) | 0.76732 (18) | 0.60776 (19) | 0.0383 (7) | |
H9A | 0.371958 | 0.749761 | 0.602880 | 0.057* | |
H9B | 0.430228 | 0.804880 | 0.652582 | 0.057* | |
H9C | 0.443697 | 0.722728 | 0.619133 | 0.057* | |
C10 | 0.29033 (17) | 0.7455 (2) | 0.2992 (2) | 0.0489 (9) | |
H10A | 0.273983 | 0.790570 | 0.319801 | 0.073* | |
H10B | 0.254933 | 0.710651 | 0.270487 | 0.073* | |
H10C | 0.311072 | 0.762878 | 0.261331 | 0.073* | |
C11 | 0.30752 (17) | 0.6617 (2) | 0.4580 (2) | 0.0455 (8) | |
H11A | 0.337589 | 0.634616 | 0.505253 | 0.068* | |
H11B | 0.272266 | 0.626814 | 0.428917 | 0.068* | |
H11C | 0.290734 | 0.707547 | 0.476773 | 0.068* | |
C12 | 0.36677 (19) | 0.5996 (2) | 0.3437 (3) | 0.0561 (10) | |
H12A | 0.378534 | 0.610788 | 0.295846 | 0.084* | |
H12B | 0.328708 | 0.566634 | 0.327294 | 0.084* | |
H12C | 0.402040 | 0.572692 | 0.385153 | 0.084* | |
C13 | 0.58808 (17) | 1.04898 (18) | 0.2724 (2) | 0.0416 (7) | |
H13A | 0.576298 | 1.053510 | 0.321741 | 0.050* | |
H13B | 0.566101 | 1.090399 | 0.233316 | 0.050* | |
C14 | 0.65940 (19) | 1.0549 (2) | 0.2947 (2) | 0.0547 (9) | |
H14A | 0.682001 | 1.036790 | 0.351398 | 0.066* | |
H14B | 0.672380 | 1.108948 | 0.289447 | 0.066* | |
C15 | 0.6732 (2) | 1.0019 (3) | 0.2329 (3) | 0.0830 (16) | |
H15A | 0.686751 | 1.032568 | 0.194063 | 0.100* | |
H15B | 0.707222 | 0.964249 | 0.261184 | 0.100* | |
C16 | 0.61219 (17) | 0.9610 (2) | 0.1894 (2) | 0.0478 (8) | |
H16A | 0.592302 | 0.981604 | 0.133204 | 0.057* | |
H16B | 0.619827 | 0.904706 | 0.185990 | 0.057* | |
C17 | 0.6185 (2) | 0.5338 (2) | 0.3979 (2) | 0.0565 (10) | |
H17A | 0.610593 | 0.502048 | 0.440596 | 0.068* | |
H17B | 0.619886 | 0.589213 | 0.413246 | 0.068* | |
C18 | 0.68020 (19) | 0.5094 (2) | 0.3867 (2) | 0.0559 (10) | |
H18A | 0.712452 | 0.492711 | 0.439224 | 0.067* | |
H18B | 0.697985 | 0.552445 | 0.363767 | 0.067* | |
C19 | 0.65973 (17) | 0.4419 (2) | 0.3265 (2) | 0.0440 (8) | |
H19A | 0.677828 | 0.447050 | 0.282646 | 0.053* | |
H19B | 0.673445 | 0.391682 | 0.354859 | 0.053* | |
C20 | 0.58746 (18) | 0.44804 (19) | 0.2921 (2) | 0.0466 (8) | |
H20A | 0.571838 | 0.446523 | 0.231567 | 0.056* | |
H20B | 0.568085 | 0.404319 | 0.311814 | 0.056* | |
H1 | 0.4847 (15) | 0.8127 (18) | 0.345 (2) | 0.031 (8)* | |
H2 | 0.4846 (16) | 0.675 (2) | 0.352 (2) | 0.040 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.0297 (4) | 0.0277 (4) | 0.0201 (4) | 0.0006 (3) | 0.0082 (3) | 0.0000 (3) |
Na1 | 0.0435 (9) | 0.0274 (8) | 0.0309 (8) | 0.000 | 0.0187 (7) | 0.000 |
Na2 | 0.0473 (9) | 0.0281 (8) | 0.0283 (8) | 0.000 | 0.0151 (7) | 0.000 |
Si1 | 0.0308 (4) | 0.0300 (4) | 0.0274 (4) | −0.0012 (3) | 0.0095 (3) | −0.0007 (3) |
Si2 | 0.0366 (4) | 0.0265 (4) | 0.0225 (4) | 0.0019 (3) | 0.0061 (3) | 0.0009 (3) |
Si3 | 0.0357 (4) | 0.0267 (4) | 0.0257 (4) | −0.0001 (3) | 0.0136 (3) | −0.0004 (3) |
Si4 | 0.0328 (4) | 0.0362 (4) | 0.0271 (4) | −0.0059 (3) | 0.0104 (3) | −0.0030 (3) |
O1 | 0.0474 (12) | 0.0336 (11) | 0.0384 (11) | −0.0096 (9) | 0.0230 (10) | −0.0095 (9) |
O2 | 0.0650 (15) | 0.0355 (12) | 0.0296 (11) | 0.0125 (11) | 0.0068 (11) | −0.0034 (9) |
N1 | 0.0304 (12) | 0.0254 (11) | 0.0233 (11) | 0.0006 (9) | 0.0066 (9) | −0.0015 (9) |
N2 | 0.0311 (12) | 0.0282 (12) | 0.0251 (11) | −0.0005 (9) | 0.0112 (9) | −0.0017 (9) |
C1 | 0.0455 (17) | 0.0330 (15) | 0.0416 (17) | −0.0058 (13) | 0.0211 (14) | −0.0023 (13) |
C2 | 0.0349 (16) | 0.051 (2) | 0.0397 (17) | −0.0068 (14) | 0.0070 (14) | −0.0024 (15) |
C3 | 0.0376 (16) | 0.0440 (17) | 0.0347 (16) | 0.0012 (13) | 0.0153 (13) | 0.0000 (13) |
C4 | 0.0468 (18) | 0.0362 (16) | 0.0388 (17) | 0.0084 (14) | 0.0041 (14) | 0.0016 (14) |
C5 | 0.0502 (18) | 0.0381 (16) | 0.0264 (14) | 0.0025 (14) | 0.0098 (13) | 0.0010 (12) |
C6 | 0.0495 (18) | 0.0304 (15) | 0.0308 (15) | 0.0004 (13) | 0.0085 (13) | 0.0058 (12) |
C7 | 0.0410 (16) | 0.0289 (14) | 0.0304 (14) | 0.0016 (12) | 0.0140 (12) | −0.0028 (11) |
C8 | 0.0416 (16) | 0.0325 (15) | 0.0406 (17) | 0.0025 (12) | 0.0202 (14) | 0.0013 (13) |
C9 | 0.0524 (19) | 0.0352 (16) | 0.0301 (15) | −0.0031 (14) | 0.0181 (14) | −0.0023 (12) |
C10 | 0.0423 (18) | 0.067 (2) | 0.0322 (16) | −0.0094 (16) | 0.0064 (14) | 0.0048 (16) |
C11 | 0.0462 (18) | 0.0499 (19) | 0.0401 (17) | −0.0147 (15) | 0.0149 (15) | 0.0023 (15) |
C12 | 0.052 (2) | 0.053 (2) | 0.065 (2) | −0.0180 (17) | 0.0216 (19) | −0.0270 (19) |
C13 | 0.058 (2) | 0.0323 (16) | 0.0363 (16) | −0.0070 (14) | 0.0192 (15) | −0.0071 (13) |
C14 | 0.060 (2) | 0.057 (2) | 0.045 (2) | −0.0206 (18) | 0.0154 (17) | −0.0109 (17) |
C15 | 0.059 (3) | 0.118 (4) | 0.082 (3) | −0.036 (3) | 0.037 (2) | −0.047 (3) |
C16 | 0.054 (2) | 0.050 (2) | 0.050 (2) | −0.0118 (16) | 0.0316 (17) | −0.0158 (16) |
C17 | 0.083 (3) | 0.0425 (19) | 0.0300 (16) | 0.0085 (19) | 0.0029 (17) | −0.0066 (14) |
C18 | 0.064 (2) | 0.045 (2) | 0.044 (2) | −0.0110 (18) | 0.0012 (17) | 0.0013 (16) |
C19 | 0.055 (2) | 0.0398 (17) | 0.0394 (17) | 0.0007 (15) | 0.0191 (15) | 0.0029 (14) |
C20 | 0.058 (2) | 0.0321 (16) | 0.0445 (18) | 0.0053 (15) | 0.0115 (16) | −0.0073 (14) |
Al1—N2 | 1.872 (2) | C5—H5C | 0.9800 |
Al1—N1 | 1.876 (2) | C6—H6A | 0.9800 |
Al1—H1 | 1.55 (3) | C6—H6B | 0.9800 |
Al1—H2 | 1.53 (3) | C6—H6C | 0.9800 |
Na1—O1i | 2.279 (2) | C7—H7A | 0.9800 |
Na1—O1 | 2.279 (2) | C7—H7B | 0.9800 |
Na1—H1 | 2.21 (3) | C7—H7C | 0.9800 |
Na2—O2 | 2.264 (2) | C8—H8A | 0.9800 |
Na2—O2i | 2.264 (2) | C8—H8B | 0.9800 |
Na2—H2 | 2.21 (3) | C8—H8C | 0.9800 |
Si1—N1 | 1.719 (2) | C9—H9A | 0.9800 |
Si1—C2 | 1.875 (3) | C9—H9B | 0.9800 |
Si1—C3 | 1.880 (3) | C9—H9C | 0.9800 |
Si1—C1 | 1.880 (3) | C10—H10A | 0.9800 |
Si2—N1 | 1.725 (2) | C10—H10B | 0.9800 |
Si2—C6 | 1.875 (3) | C10—H10C | 0.9800 |
Si2—C5 | 1.880 (3) | C11—H11A | 0.9800 |
Si2—C4 | 1.887 (3) | C11—H11B | 0.9800 |
Si3—N2 | 1.729 (2) | C11—H11C | 0.9800 |
Si3—C7 | 1.870 (3) | C12—H12A | 0.9800 |
Si3—C9 | 1.883 (3) | C12—H12B | 0.9800 |
Si3—C8 | 1.884 (3) | C12—H12C | 0.9800 |
Si4—N2 | 1.725 (2) | C13—C14 | 1.509 (5) |
Si4—C12 | 1.870 (4) | C13—H13A | 0.9900 |
Si4—C10 | 1.875 (4) | C13—H13B | 0.9900 |
Si4—C11 | 1.879 (3) | C14—C15 | 1.526 (6) |
O1—C13 | 1.428 (4) | C14—H14A | 0.9900 |
O1—C16 | 1.436 (4) | C14—H14B | 0.9900 |
O2—C17 | 1.425 (4) | C15—C16 | 1.486 (5) |
O2—C20 | 1.430 (4) | C15—H15A | 0.9900 |
C1—H1A | 0.9800 | C15—H15B | 0.9900 |
C1—H1B | 0.9800 | C16—H16A | 0.9900 |
C1—H1C | 0.9800 | C16—H16B | 0.9900 |
C2—H2A | 0.9800 | C17—C18 | 1.522 (6) |
C2—H2B | 0.9800 | C17—H17A | 0.9900 |
C2—H2C | 0.9800 | C17—H17B | 0.9900 |
C3—H3A | 0.9800 | C18—C19 | 1.526 (5) |
C3—H3B | 0.9800 | C18—H18A | 0.9900 |
C3—H3C | 0.9800 | C18—H18B | 0.9900 |
C4—H4A | 0.9800 | C19—C20 | 1.519 (5) |
C4—H4B | 0.9800 | C19—H19A | 0.9900 |
C4—H4C | 0.9800 | C19—H19B | 0.9900 |
C5—H5A | 0.9800 | C20—H20A | 0.9900 |
C5—H5B | 0.9800 | C20—H20B | 0.9900 |
N2—Al1—N1 | 118.28 (11) | Si3—C7—H7A | 109.5 |
N2—Al1—H1 | 110.6 (12) | Si3—C7—H7B | 109.5 |
N1—Al1—H1 | 106.6 (12) | H7A—C7—H7B | 109.5 |
N2—Al1—H2 | 110.3 (13) | Si3—C7—H7C | 109.5 |
N1—Al1—H2 | 108.1 (13) | H7A—C7—H7C | 109.5 |
H1—Al1—H2 | 101.6 (18) | H7B—C7—H7C | 109.5 |
O1i—Na1—O1 | 96.84 (12) | Si3—C8—H8A | 109.5 |
O1i—Na1—H1 | 89.9 (8) | Si3—C8—H8B | 109.5 |
O1—Na1—H1 | 139.9 (8) | H8A—C8—H8B | 109.5 |
O2—Na2—O2i | 91.72 (13) | Si3—C8—H8C | 109.5 |
O2—Na2—H2 | 100.9 (9) | H8A—C8—H8C | 109.5 |
O2i—Na2—H2 | 119.6 (9) | H8B—C8—H8C | 109.5 |
N1—Si1—C2 | 113.95 (14) | Si3—C9—H9A | 109.5 |
N1—Si1—C3 | 110.44 (13) | Si3—C9—H9B | 109.5 |
C2—Si1—C3 | 106.93 (15) | H9A—C9—H9B | 109.5 |
N1—Si1—C1 | 115.13 (13) | Si3—C9—H9C | 109.5 |
C2—Si1—C1 | 102.73 (16) | H9A—C9—H9C | 109.5 |
C3—Si1—C1 | 107.01 (15) | H9B—C9—H9C | 109.5 |
N1—Si2—C6 | 109.80 (13) | Si4—C10—H10A | 109.5 |
N1—Si2—C5 | 112.13 (13) | Si4—C10—H10B | 109.5 |
C6—Si2—C5 | 108.71 (15) | H10A—C10—H10B | 109.5 |
N1—Si2—C4 | 115.34 (14) | Si4—C10—H10C | 109.5 |
C6—Si2—C4 | 105.94 (15) | H10A—C10—H10C | 109.5 |
C5—Si2—C4 | 104.53 (15) | H10B—C10—H10C | 109.5 |
N2—Si3—C7 | 111.99 (12) | Si4—C11—H11A | 109.5 |
N2—Si3—C9 | 112.70 (13) | Si4—C11—H11B | 109.5 |
C7—Si3—C9 | 107.18 (14) | H11A—C11—H11B | 109.5 |
N2—Si3—C8 | 113.25 (13) | Si4—C11—H11C | 109.5 |
C7—Si3—C8 | 105.15 (14) | H11A—C11—H11C | 109.5 |
C9—Si3—C8 | 106.02 (15) | H11B—C11—H11C | 109.5 |
N2—Si4—C12 | 114.68 (14) | Si4—C12—H12A | 109.5 |
N2—Si4—C10 | 112.34 (14) | Si4—C12—H12B | 109.5 |
C12—Si4—C10 | 105.76 (19) | H12A—C12—H12B | 109.5 |
N2—Si4—C11 | 111.61 (14) | Si4—C12—H12C | 109.5 |
C12—Si4—C11 | 104.32 (18) | H12A—C12—H12C | 109.5 |
C10—Si4—C11 | 107.54 (17) | H12B—C12—H12C | 109.5 |
C13—O1—C16 | 106.2 (2) | O1—C13—C14 | 105.2 (3) |
C13—O1—Na1 | 129.20 (19) | O1—C13—H13A | 110.7 |
C16—O1—Na1 | 124.55 (19) | C14—C13—H13A | 110.7 |
C17—O2—C20 | 105.6 (3) | O1—C13—H13B | 110.7 |
C17—O2—Na2 | 123.2 (2) | C14—C13—H13B | 110.7 |
C20—O2—Na2 | 129.9 (2) | H13A—C13—H13B | 108.8 |
Si1—N1—Si2 | 124.23 (14) | C13—C14—C15 | 103.7 (3) |
Si1—N1—Al1 | 114.88 (13) | C13—C14—H14A | 111.0 |
Si2—N1—Al1 | 120.35 (13) | C15—C14—H14A | 111.0 |
Si4—N2—Si3 | 118.29 (14) | C13—C14—H14B | 111.0 |
Si4—N2—Al1 | 120.69 (13) | C15—C14—H14B | 111.0 |
Si3—N2—Al1 | 120.60 (13) | H14A—C14—H14B | 109.0 |
Si1—C1—H1A | 109.5 | C16—C15—C14 | 105.5 (3) |
Si1—C1—H1B | 109.5 | C16—C15—H15A | 110.6 |
H1A—C1—H1B | 109.5 | C14—C15—H15A | 110.7 |
Si1—C1—H1C | 109.5 | C16—C15—H15B | 110.6 |
H1A—C1—H1C | 109.5 | C14—C15—H15B | 110.6 |
H1B—C1—H1C | 109.5 | H15A—C15—H15B | 108.8 |
Si1—C2—H2A | 109.5 | O1—C16—C15 | 106.8 (3) |
Si1—C2—H2B | 109.5 | O1—C16—H16A | 110.4 |
H2A—C2—H2B | 109.5 | C15—C16—H16A | 110.4 |
Si1—C2—H2C | 109.5 | O1—C16—H16B | 110.4 |
H2A—C2—H2C | 109.5 | C15—C16—H16B | 110.4 |
H2B—C2—H2C | 109.5 | H16A—C16—H16B | 108.6 |
Si1—C3—H3A | 109.5 | O2—C17—C18 | 103.8 (3) |
Si1—C3—H3B | 109.5 | O2—C17—H17A | 111.0 |
H3A—C3—H3B | 109.5 | C18—C17—H17A | 111.0 |
Si1—C3—H3C | 109.5 | O2—C17—H17B | 111.0 |
H3A—C3—H3C | 109.5 | C18—C17—H17B | 111.0 |
H3B—C3—H3C | 109.5 | H17A—C17—H17B | 109.0 |
Si2—C4—H4A | 109.5 | C17—C18—C19 | 103.4 (3) |
Si2—C4—H4B | 109.5 | C17—C18—H18A | 111.1 |
H4A—C4—H4B | 109.5 | C19—C18—H18A | 111.1 |
Si2—C4—H4C | 109.5 | C17—C18—H18B | 111.1 |
H4A—C4—H4C | 109.5 | C19—C18—H18B | 111.1 |
H4B—C4—H4C | 109.5 | H18A—C18—H18B | 109.0 |
Si2—C5—H5A | 109.5 | C20—C19—C18 | 103.8 (3) |
Si2—C5—H5B | 109.5 | C20—C19—H19A | 111.0 |
H5A—C5—H5B | 109.5 | C18—C19—H19A | 111.0 |
Si2—C5—H5C | 109.5 | C20—C19—H19B | 111.0 |
H5A—C5—H5C | 109.5 | C18—C19—H19B | 111.0 |
H5B—C5—H5C | 109.5 | H19A—C19—H19B | 109.0 |
Si2—C6—H6A | 109.5 | O2—C20—C19 | 107.2 (3) |
Si2—C6—H6B | 109.5 | O2—C20—H20A | 110.3 |
H6A—C6—H6B | 109.5 | C19—C20—H20A | 110.3 |
Si2—C6—H6C | 109.5 | O2—C20—H20B | 110.3 |
H6A—C6—H6C | 109.5 | C19—C20—H20B | 110.3 |
H6B—C6—H6C | 109.5 | H20A—C20—H20B | 108.5 |
C2—Si1—N1—Si2 | −8.5 (2) | C9—Si3—N2—Si4 | 74.85 (19) |
C3—Si1—N1—Si2 | 111.87 (18) | C8—Si3—N2—Si4 | −45.49 (19) |
C1—Si1—N1—Si2 | −126.83 (17) | C7—Si3—N2—Al1 | 8.37 (19) |
C2—Si1—N1—Al1 | −179.99 (15) | C9—Si3—N2—Al1 | −112.58 (17) |
C3—Si1—N1—Al1 | −59.62 (17) | C8—Si3—N2—Al1 | 127.07 (16) |
C1—Si1—N1—Al1 | 61.68 (18) | N1—Al1—N2—Si4 | −141.53 (14) |
C6—Si2—N1—Si1 | −159.84 (16) | N1—Al1—N2—Si3 | 46.08 (18) |
C5—Si2—N1—Si1 | 79.2 (2) | C16—O1—C13—C14 | −36.7 (3) |
C4—Si2—N1—Si1 | −40.3 (2) | Na1—O1—C13—C14 | 139.8 (2) |
C6—Si2—N1—Al1 | 11.22 (19) | O1—C13—C14—C15 | 27.3 (4) |
C5—Si2—N1—Al1 | −109.74 (17) | C13—C14—C15—C16 | −8.4 (5) |
C4—Si2—N1—Al1 | 130.78 (16) | C13—O1—C16—C15 | 31.3 (4) |
N2—Al1—N1—Si1 | −136.46 (13) | Na1—O1—C16—C15 | −145.4 (3) |
N2—Al1—N1—Si2 | 51.68 (18) | C14—C15—C16—O1 | −13.2 (5) |
C12—Si4—N2—Si3 | −157.14 (19) | C20—O2—C17—C18 | 41.2 (4) |
C10—Si4—N2—Si3 | 82.1 (2) | Na2—O2—C17—C18 | −126.9 (3) |
C11—Si4—N2—Si3 | −38.8 (2) | O2—C17—C18—C19 | −34.2 (4) |
C12—Si4—N2—Al1 | 30.3 (2) | C17—C18—C19—C20 | 14.7 (4) |
C10—Si4—N2—Al1 | −90.49 (19) | C17—O2—C20—C19 | −31.9 (4) |
C11—Si4—N2—Al1 | 148.64 (17) | Na2—O2—C20—C19 | 135.1 (3) |
C7—Si3—N2—Si4 | −164.19 (14) | C18—C19—C20—O2 | 9.4 (4) |
Symmetry code: (i) −x+1, y, −z+1/2. |
[Al2Na2(C6H18NSi2)2H6(C9H23N3)2] | Z = 1 |
Mr = 773.38 | F(000) = 428 |
Triclinic, P1 | Dx = 1.000 Mg m−3 |
a = 9.2634 (5) Å | Cu Kα radiation, λ = 1.54184 Å |
b = 11.7188 (7) Å | Cell parameters from 6113 reflections |
c = 12.6742 (7) Å | θ = 3.6–72.8° |
α = 84.811 (5)° | µ = 1.77 mm−1 |
β = 76.840 (5)° | T = 123 K |
γ = 73.485 (5)° | Fragment, colourless |
V = 1283.97 (13) Å3 | 0.44 × 0.20 × 0.10 mm |
Oxford Diffraction Gemini S diffractometer | 4511 reflections with I > 2σ(I) |
Radiation source: sealed tube | Rint = 0.028 |
ω scans | θmax = 73.1°, θmin = 5.5° |
Absorption correction: multi-scan (CrysalisPro; Rigaku OD, 2021) | h = −11→11 |
Tmin = 0.256, Tmax = 1.000 | k = −11→14 |
14891 measured reflections | l = −12→15 |
5082 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.040 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.112 | w = 1/[σ2(Fo2) + (0.0708P)2 + 0.2717P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
5082 reflections | Δρmax = 0.46 e Å−3 |
231 parameters | Δρmin = −0.21 e Å−3 |
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 | ||
Al1 | 0.15640 (5) | 0.36454 (4) | 0.86299 (3) | 0.02993 (13) | |
Na1 | 0.09543 (6) | 0.64121 (5) | 0.89017 (4) | 0.02873 (14) | |
Si1 | 0.42221 (5) | 0.17657 (4) | 0.74287 (3) | 0.03074 (12) | |
Si2 | 0.14772 (5) | 0.27561 (3) | 0.63862 (3) | 0.02898 (12) | |
N1 | 0.24175 (14) | 0.27040 (11) | 0.74157 (9) | 0.0276 (3) | |
N2 | 0.26670 (16) | 0.73937 (13) | 0.94714 (12) | 0.0381 (3) | |
N3 | 0.27235 (15) | 0.68367 (12) | 0.71937 (11) | 0.0343 (3) | |
N4 | −0.06952 (15) | 0.78444 (12) | 0.78285 (10) | 0.0328 (3) | |
C1 | 0.5770 (2) | 0.25579 (18) | 0.70459 (16) | 0.0483 (4) | |
H1A | 0.579864 | 0.288836 | 0.630531 | 0.072* | |
H1B | 0.676842 | 0.199529 | 0.708484 | 0.072* | |
H1C | 0.555328 | 0.320433 | 0.754724 | 0.072* | |
C2 | 0.4294 (2) | 0.10732 (15) | 0.88131 (12) | 0.0378 (3) | |
H2A | 0.411673 | 0.169625 | 0.933088 | 0.057* | |
H2B | 0.530737 | 0.050992 | 0.880031 | 0.057* | |
H2C | 0.349417 | 0.065084 | 0.903260 | 0.057* | |
C3 | 0.4802 (2) | 0.04831 (17) | 0.64892 (15) | 0.0527 (5) | |
H3A | 0.410822 | −0.002798 | 0.672664 | 0.079* | |
H3B | 0.586164 | 0.002034 | 0.650097 | 0.079* | |
H3C | 0.473813 | 0.078871 | 0.575073 | 0.079* | |
C4 | 0.0921 (3) | 0.13492 (17) | 0.63057 (16) | 0.0502 (5) | |
H4A | 0.184058 | 0.071871 | 0.600817 | 0.075* | |
H4B | 0.017955 | 0.149016 | 0.583416 | 0.075* | |
H4C | 0.045187 | 0.110525 | 0.703285 | 0.075* | |
C5 | −0.0369 (2) | 0.39697 (18) | 0.65368 (16) | 0.0487 (4) | |
H5A | −0.104651 | 0.386287 | 0.723284 | 0.073* | |
H5B | −0.087694 | 0.393827 | 0.594517 | 0.073* | |
H5C | −0.015061 | 0.474356 | 0.651117 | 0.073* | |
C6 | 0.2679 (2) | 0.30358 (17) | 0.50353 (12) | 0.0426 (4) | |
H6A | 0.296001 | 0.377881 | 0.504980 | 0.064* | |
H6B | 0.208877 | 0.310035 | 0.447118 | 0.064* | |
H6C | 0.361578 | 0.237430 | 0.487899 | 0.064* | |
C7 | 0.3711 (3) | 0.63945 (18) | 0.99332 (18) | 0.0560 (5) | |
H7A | 0.313825 | 0.609207 | 1.059452 | 0.084* | |
H7B | 0.453733 | 0.666266 | 1.010827 | 0.084* | |
H7C | 0.415752 | 0.575918 | 0.940628 | 0.084* | |
C8 | 0.1932 (2) | 0.83010 (18) | 1.02912 (16) | 0.0502 (5) | |
H8A | 0.120914 | 0.896553 | 0.999502 | 0.075* | |
H8B | 0.272045 | 0.859085 | 1.049613 | 0.075* | |
H8C | 0.137252 | 0.795444 | 1.093150 | 0.075* | |
C9 | 0.3473 (2) | 0.79147 (16) | 0.85071 (16) | 0.0439 (4) | |
H9A | 0.438541 | 0.808004 | 0.867603 | 0.053* | |
H9B | 0.278316 | 0.868415 | 0.832065 | 0.053* | |
C10 | 0.39983 (19) | 0.71209 (17) | 0.75246 (16) | 0.0450 (4) | |
H10A | 0.454667 | 0.752530 | 0.690948 | 0.054* | |
H10B | 0.473652 | 0.636979 | 0.769557 | 0.054* | |
C11 | 0.3315 (2) | 0.57993 (16) | 0.64911 (14) | 0.0450 (4) | |
H11A | 0.381879 | 0.510420 | 0.689467 | 0.067* | |
H11B | 0.406052 | 0.596702 | 0.585539 | 0.067* | |
H11C | 0.245788 | 0.563578 | 0.625543 | 0.067* | |
C12 | 0.1830 (2) | 0.78566 (15) | 0.66357 (13) | 0.0402 (4) | |
H12A | 0.235289 | 0.787619 | 0.586317 | 0.048* | |
H12B | 0.180042 | 0.860256 | 0.695995 | 0.048* | |
C13 | 0.0192 (2) | 0.77997 (16) | 0.67094 (13) | 0.0412 (4) | |
H13A | −0.033492 | 0.847476 | 0.628251 | 0.049* | |
H13B | 0.022212 | 0.705336 | 0.638558 | 0.049* | |
C14 | −0.1103 (2) | 0.90356 (15) | 0.82598 (14) | 0.0418 (4) | |
H14A | −0.171600 | 0.904038 | 0.900064 | 0.063* | |
H14B | −0.170571 | 0.960760 | 0.780285 | 0.063* | |
H14C | −0.016190 | 0.925779 | 0.826504 | 0.063* | |
C15 | −0.20954 (19) | 0.74745 (17) | 0.78988 (15) | 0.0432 (4) | |
H15A | −0.181785 | 0.665877 | 0.764622 | 0.065* | |
H15B | −0.273938 | 0.801054 | 0.744417 | 0.065* | |
H15C | −0.266747 | 0.750616 | 0.865291 | 0.065* | |
H1 | 0.027 (3) | 0.484 (2) | 0.8479 (18) | 0.057 (6)* | |
H2 | 0.281 (3) | 0.411 (2) | 0.899 (2) | 0.067 (7)* | |
H3 | 0.080 (3) | 0.296 (2) | 0.9634 (18) | 0.056 (6)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Al1 | 0.0318 (2) | 0.0301 (2) | 0.0260 (2) | −0.00858 (17) | 0.00097 (17) | −0.00846 (16) |
Na1 | 0.0294 (3) | 0.0304 (3) | 0.0252 (3) | −0.0080 (2) | −0.0028 (2) | −0.0030 (2) |
Si1 | 0.0321 (2) | 0.0321 (2) | 0.0228 (2) | −0.00108 (16) | −0.00370 (15) | −0.00400 (15) |
Si2 | 0.0335 (2) | 0.0311 (2) | 0.0230 (2) | −0.00925 (16) | −0.00644 (15) | −0.00147 (15) |
N1 | 0.0313 (6) | 0.0284 (6) | 0.0211 (5) | −0.0040 (5) | −0.0052 (4) | −0.0049 (4) |
N2 | 0.0344 (7) | 0.0400 (7) | 0.0415 (7) | −0.0082 (6) | −0.0098 (6) | −0.0105 (6) |
N3 | 0.0327 (7) | 0.0318 (6) | 0.0328 (6) | −0.0066 (5) | 0.0036 (5) | −0.0059 (5) |
N4 | 0.0312 (6) | 0.0363 (7) | 0.0276 (6) | −0.0036 (5) | −0.0056 (5) | −0.0046 (5) |
C1 | 0.0310 (8) | 0.0525 (10) | 0.0522 (10) | −0.0063 (7) | 0.0006 (7) | 0.0053 (8) |
C2 | 0.0414 (9) | 0.0400 (8) | 0.0291 (7) | −0.0039 (7) | −0.0116 (6) | 0.0013 (6) |
C3 | 0.0617 (12) | 0.0434 (10) | 0.0405 (9) | 0.0130 (8) | −0.0141 (8) | −0.0172 (8) |
C4 | 0.0692 (13) | 0.0476 (10) | 0.0451 (10) | −0.0302 (9) | −0.0165 (9) | −0.0012 (8) |
C5 | 0.0395 (9) | 0.0555 (11) | 0.0491 (10) | −0.0008 (8) | −0.0188 (8) | −0.0063 (8) |
C6 | 0.0528 (10) | 0.0518 (10) | 0.0231 (7) | −0.0163 (8) | −0.0065 (7) | 0.0021 (7) |
C7 | 0.0612 (12) | 0.0476 (10) | 0.0642 (13) | −0.0052 (9) | −0.0323 (10) | −0.0097 (9) |
C8 | 0.0482 (10) | 0.0535 (11) | 0.0515 (10) | −0.0103 (8) | −0.0133 (8) | −0.0203 (9) |
C9 | 0.0315 (8) | 0.0439 (9) | 0.0580 (11) | −0.0140 (7) | −0.0046 (7) | −0.0108 (8) |
C10 | 0.0292 (8) | 0.0486 (10) | 0.0523 (10) | −0.0114 (7) | 0.0057 (7) | −0.0101 (8) |
C11 | 0.0474 (10) | 0.0380 (9) | 0.0401 (9) | −0.0077 (7) | 0.0085 (7) | −0.0112 (7) |
C12 | 0.0468 (9) | 0.0357 (8) | 0.0299 (7) | −0.0092 (7) | 0.0051 (7) | 0.0008 (6) |
C13 | 0.0470 (9) | 0.0447 (9) | 0.0261 (7) | −0.0032 (7) | −0.0071 (7) | −0.0027 (6) |
C14 | 0.0399 (9) | 0.0393 (9) | 0.0397 (9) | −0.0020 (7) | −0.0042 (7) | −0.0066 (7) |
C15 | 0.0334 (8) | 0.0513 (10) | 0.0445 (9) | −0.0061 (7) | −0.0117 (7) | −0.0082 (8) |
Al1—N1 | 1.8621 (12) | C3—H3C | 0.9800 |
Al1—Na1i | 3.4586 (7) | C4—H4A | 0.9800 |
Al1—H1 | 1.59 (2) | C4—H4B | 0.9800 |
Al1—H2 | 1.57 (3) | C4—H4C | 0.9800 |
Al1—H3 | 1.58 (2) | C5—H5A | 0.9800 |
Na1—N2 | 2.4639 (15) | C5—H5B | 0.9800 |
Na1—N4 | 2.4651 (14) | C5—H5C | 0.9800 |
Na1—N3 | 2.5046 (14) | C6—H6A | 0.9800 |
Na1—H1 | 2.25 (2) | C6—H6B | 0.9800 |
H3—Na1i | 2.20 (2) | C6—H6C | 0.9800 |
Si1—N1 | 1.7229 (13) | C7—H7A | 0.9800 |
Si1—C2 | 1.8726 (16) | C7—H7B | 0.9800 |
Si1—C1 | 1.8742 (19) | C7—H7C | 0.9800 |
Si1—C3 | 1.8812 (17) | C8—H8A | 0.9800 |
Si2—N1 | 1.7140 (12) | C8—H8B | 0.9800 |
Si2—C5 | 1.8713 (18) | C8—H8C | 0.9800 |
Si2—C6 | 1.8751 (17) | C9—C10 | 1.526 (2) |
Si2—C4 | 1.8793 (18) | C9—H9A | 0.9900 |
N2—C9 | 1.460 (2) | C9—H9B | 0.9900 |
N2—C7 | 1.463 (2) | C10—H10A | 0.9900 |
N2—C8 | 1.463 (2) | C10—H10B | 0.9900 |
N3—C10 | 1.468 (2) | C11—H11A | 0.9800 |
N3—C12 | 1.471 (2) | C11—H11B | 0.9800 |
N3—C11 | 1.472 (2) | C11—H11C | 0.9800 |
N4—C14 | 1.461 (2) | C12—C13 | 1.519 (3) |
N4—C15 | 1.462 (2) | C12—H12A | 0.9900 |
N4—C13 | 1.4656 (19) | C12—H12B | 0.9900 |
C1—H1A | 0.9800 | C13—H13A | 0.9900 |
C1—H1B | 0.9800 | C13—H13B | 0.9900 |
C1—H1C | 0.9800 | C14—H14A | 0.9800 |
C2—H2A | 0.9800 | C14—H14B | 0.9800 |
C2—H2B | 0.9800 | C14—H14C | 0.9800 |
C2—H2C | 0.9800 | C15—H15A | 0.9800 |
C3—H3A | 0.9800 | C15—H15B | 0.9800 |
C3—H3B | 0.9800 | C15—H15C | 0.9800 |
N1—Al1—Na1i | 138.06 (4) | Si2—C4—H4B | 109.5 |
N1—Al1—H1 | 115.9 (8) | H4A—C4—H4B | 109.5 |
Na1i—Al1—H1 | 81.2 (8) | Si2—C4—H4C | 109.5 |
N1—Al1—H2 | 111.6 (9) | H4A—C4—H4C | 109.5 |
Na1i—Al1—H2 | 100.0 (9) | H4B—C4—H4C | 109.5 |
H1—Al1—H2 | 102.9 (12) | Si2—C5—H5A | 109.5 |
N1—Al1—H3 | 112.5 (8) | Si2—C5—H5B | 109.5 |
Na1i—Al1—H3 | 28.2 (8) | H5A—C5—H5B | 109.5 |
H1—Al1—H3 | 105.5 (11) | Si2—C5—H5C | 109.5 |
H2—Al1—H3 | 107.7 (12) | H5A—C5—H5C | 109.5 |
N2—Na1—N4 | 109.15 (5) | H5B—C5—H5C | 109.5 |
N2—Na1—N3 | 74.35 (5) | Si2—C6—H6A | 109.5 |
N4—Na1—N3 | 74.05 (5) | Si2—C6—H6B | 109.5 |
N2—Na1—Al1i | 98.40 (4) | H6A—C6—H6B | 109.5 |
N4—Na1—Al1i | 101.98 (4) | Si2—C6—H6C | 109.5 |
N3—Na1—Al1i | 169.57 (4) | H6A—C6—H6C | 109.5 |
N2—Na1—H1 | 154.8 (6) | H6B—C6—H6C | 109.5 |
N4—Na1—H1 | 93.8 (6) | N2—C7—H7A | 109.5 |
N3—Na1—H1 | 103.3 (6) | N2—C7—H7B | 109.5 |
Al1i—Na1—H1 | 86.5 (6) | H7A—C7—H7B | 109.5 |
N1—Si1—C2 | 110.28 (7) | N2—C7—H7C | 109.5 |
N1—Si1—C1 | 112.43 (7) | H7A—C7—H7C | 109.5 |
C2—Si1—C1 | 107.83 (9) | H7B—C7—H7C | 109.5 |
N1—Si1—C3 | 113.92 (8) | N2—C8—H8A | 109.5 |
C2—Si1—C3 | 105.48 (8) | N2—C8—H8B | 109.5 |
C1—Si1—C3 | 106.49 (10) | H8A—C8—H8B | 109.5 |
N1—Si2—C5 | 112.92 (7) | N2—C8—H8C | 109.5 |
N1—Si2—C6 | 111.60 (7) | H8A—C8—H8C | 109.5 |
C5—Si2—C6 | 106.10 (9) | H8B—C8—H8C | 109.5 |
N1—Si2—C4 | 112.80 (8) | N2—C9—C10 | 113.56 (14) |
C5—Si2—C4 | 105.06 (10) | N2—C9—H9A | 108.9 |
C6—Si2—C4 | 107.88 (9) | C10—C9—H9A | 108.9 |
Si2—N1—Si1 | 123.12 (7) | N2—C9—H9B | 108.9 |
Si2—N1—Al1 | 122.84 (7) | C10—C9—H9B | 108.9 |
Si1—N1—Al1 | 114.04 (6) | H9A—C9—H9B | 107.7 |
C9—N2—C7 | 111.89 (15) | N3—C10—C9 | 113.27 (13) |
C9—N2—C8 | 109.57 (15) | N3—C10—H10A | 108.9 |
C7—N2—C8 | 108.88 (15) | C9—C10—H10A | 108.9 |
C9—N2—Na1 | 108.11 (10) | N3—C10—H10B | 108.9 |
C7—N2—Na1 | 102.07 (11) | C9—C10—H10B | 108.9 |
C8—N2—Na1 | 116.18 (11) | H10A—C10—H10B | 107.7 |
C10—N3—C12 | 111.69 (14) | N3—C11—H11A | 109.5 |
C10—N3—C11 | 110.25 (13) | N3—C11—H11B | 109.5 |
C12—N3—C11 | 110.07 (14) | H11A—C11—H11B | 109.5 |
C10—N3—Na1 | 106.49 (10) | N3—C11—H11C | 109.5 |
C12—N3—Na1 | 107.15 (9) | H11A—C11—H11C | 109.5 |
C11—N3—Na1 | 111.10 (10) | H11B—C11—H11C | 109.5 |
C14—N4—C15 | 109.51 (13) | N3—C12—C13 | 112.39 (14) |
C14—N4—C13 | 111.49 (14) | N3—C12—H12A | 109.1 |
C15—N4—C13 | 110.79 (13) | C13—C12—H12A | 109.1 |
C14—N4—Na1 | 109.95 (10) | N3—C12—H12B | 109.1 |
C15—N4—Na1 | 108.44 (10) | C13—C12—H12B | 109.1 |
C13—N4—Na1 | 106.57 (9) | H12A—C12—H12B | 107.9 |
Si1—C1—H1A | 109.5 | N4—C13—C12 | 112.54 (13) |
Si1—C1—H1B | 109.5 | N4—C13—H13A | 109.1 |
H1A—C1—H1B | 109.5 | C12—C13—H13A | 109.1 |
Si1—C1—H1C | 109.5 | N4—C13—H13B | 109.1 |
H1A—C1—H1C | 109.5 | C12—C13—H13B | 109.1 |
H1B—C1—H1C | 109.5 | H13A—C13—H13B | 107.8 |
Si1—C2—H2A | 109.5 | N4—C14—H14A | 109.5 |
Si1—C2—H2B | 109.5 | N4—C14—H14B | 109.5 |
H2A—C2—H2B | 109.5 | H14A—C14—H14B | 109.5 |
Si1—C2—H2C | 109.5 | N4—C14—H14C | 109.5 |
H2A—C2—H2C | 109.5 | H14A—C14—H14C | 109.5 |
H2B—C2—H2C | 109.5 | H14B—C14—H14C | 109.5 |
Si1—C3—H3A | 109.5 | N4—C15—H15A | 109.5 |
Si1—C3—H3B | 109.5 | N4—C15—H15B | 109.5 |
H3A—C3—H3B | 109.5 | H15A—C15—H15B | 109.5 |
Si1—C3—H3C | 109.5 | N4—C15—H15C | 109.5 |
H3A—C3—H3C | 109.5 | H15A—C15—H15C | 109.5 |
H3B—C3—H3C | 109.5 | H15B—C15—H15C | 109.5 |
Si2—C4—H4A | 109.5 | ||
C5—Si2—N1—Si1 | −174.14 (9) | C7—N2—C9—C10 | 70.97 (19) |
C6—Si2—N1—Si1 | −54.71 (11) | C8—N2—C9—C10 | −168.16 (15) |
C4—Si2—N1—Si1 | 66.93 (12) | Na1—N2—C9—C10 | −40.65 (17) |
C5—Si2—N1—Al1 | 6.69 (12) | C12—N3—C10—C9 | 75.00 (19) |
C6—Si2—N1—Al1 | 126.12 (9) | C11—N3—C10—C9 | −162.28 (15) |
C4—Si2—N1—Al1 | −112.24 (10) | Na1—N3—C10—C9 | −41.67 (17) |
C2—Si1—N1—Si2 | −137.16 (9) | N2—C9—C10—N3 | 59.5 (2) |
C1—Si1—N1—Si2 | 102.47 (10) | C10—N3—C12—C13 | −155.70 (13) |
C3—Si1—N1—Si2 | −18.79 (12) | C11—N3—C12—C13 | 81.48 (16) |
C2—Si1—N1—Al1 | 42.07 (10) | Na1—N3—C12—C13 | −39.45 (15) |
C1—Si1—N1—Al1 | −78.30 (10) | C14—N4—C13—C12 | 72.82 (17) |
C3—Si1—N1—Al1 | 160.44 (9) | C15—N4—C13—C12 | −164.94 (14) |
Na1i—Al1—N1—Si2 | 82.91 (9) | Na1—N4—C13—C12 | −47.17 (16) |
Na1i—Al1—N1—Si1 | −96.33 (8) | N3—C12—C13—N4 | 62.45 (18) |
Symmetry code: (i) −x, −y+1, −z+2. |
Funding information
MTW thanks the University of Strathclyde for funding his PhD via a Research Excellence Award.
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