1,3,7,9-Tetra­kis[2,6-bis­(1-methyl­eth­yl)phen­yl]-2,2,8,8-tetra­phen­yl-5,10-di­thia-1,3,7,9-tetra­aza-2,8-disila-4,6-digermadi­spiro­[3.1.3.1]decane aceto­nitrile monosolvate

Guo, W.; Ma, F.; Zheng, W.

doi:10.1107/S2414314616002996

1,3,7,9-Tetrakis[2,6-bis(1-methylethyl)phenyl]-2,2,8,8-tetraphenyl-5,10-dithia-1,3,7,9-tetraaza-2,8-disila-4,6-digermadispiro[3.1.3.1]decane acetonitrile monosolvate

In the compound, [η²(N,N)-Ph₂Si(NDipp)₂Ge(μ-S)]₂·CH₃CN (Dipp = 2,6-iPr₂C₆H₃), C₇₂H₈₈Ge₂N₄S₂Si₂·CH₂CN, the dimeric germanethione complex lies about an inversion centre with the two Ge^IV atoms bridged by two sulfide ligands forming the central Ge₂S₂ ring. Each Ge^IV atom is also coordinated by two N atoms from the bulky bis(amido)silane ligands in a slightly distorted tetrahedral coordination geometry. An acetonitrile solvent molecule, disordered about an inversion centre, is also present.

Keywords: germanium(IV); sulfide; bis(amido)silane; germanethione dimer; crystal structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314616002996/sj4006sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2414314616002996/sj4006Isup2.hkl Contains datablock I
	Chemical Markup Language (CML) file https://doi.org/10.1107/S2414314616002996/sj4006Isup3.cml Supplementary material

CCDC reference: 1454736

checkCIF report

Key indicators

Single-crystal X-ray study
T = 153 K
Mean (C-C) = 0.008 Å
Disorder in solvent or counterion
R factor = 0.046
wR factor = 0.138
Data-to-parameter ratio = 17.3

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT934_ALERT_3_B Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          3 Check

Alert level C
PLAT220_ALERT_2_C Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        4.9 Ratio
PLAT241_ALERT_2_C High   'MainMol' Ueq as Compared to Neighbors of        C16 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of         C7 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C19 Check
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        C22 Check
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00775 Ang.
PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Th(Min) ...          9 Report

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          6 Note
PLAT005_ALERT_5_G No Embedded Refinement Details found  in the CIF     Please Do !
PLAT008_ALERT_5_G No _iucr_refine_reflections_details   in the CIF     Please Do !
PLAT066_ALERT_1_G Predicted and Reported Tmin&Tmax Range Identical          ? Check
PLAT152_ALERT_1_G The Supplied and Calc. Volume s.u. Differ by ...          2 Units
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.004 Degree
PLAT300_ALERT_4_G Atom Site Occupancy of *N3     is Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *C37    is Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *C38    is Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H38A   is Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H38B   is Constrained at        0.5 Check
PLAT300_ALERT_4_G Atom Site Occupancy of *H38C   is Constrained at        0.5 Check
PLAT302_ALERT_4_G Anion/Solvent Disorder ............ Percentage =        100 Note
PLAT432_ALERT_2_G Short Inter X...Y Contact  N3     ..  C38     ..       2.09 Ang.
PLAT432_ALERT_2_G Short Inter X...Y Contact  C37    ..  C38     ..       1.11 Ang.
PLAT432_ALERT_2_G Short Inter X...Y Contact  C37    ..  C37     ..       2.48 Ang.
PLAT432_ALERT_2_G Short Inter X...Y Contact  C38    ..  C38     ..       0.88 Ang.
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        131 Do !
            C38 -C38 -C37 -N3     45.00 39.00   2.557   1.555   1.555   1.555
PLAT710_ALERT_4_G Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #        132 Do !
            C37 -C38 -C37 -N3     45.00 39.00   2.557   1.555   1.555   1.555
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        156 Check
              C37  -C38  -H38C    2.557   1.555   1.555             39.90 Deg.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        166 Check
              N2   -GE1  -SI1     1.555   1.555   1.555             41.47 Deg.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        167 Check
              N1   -GE1  -SI1     1.555   1.555   1.555             41.92 Deg.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        183 Check
              N2   -SI1  -GE1     1.555   1.555   1.555             44.61 Deg.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        184 Check
              N1   -SI1  -GE1     1.555   1.555   1.555             44.78 Deg.
PLAT779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF .... #        189 Check
              C38  -C37  -C38     2.557   1.555   1.555             35.60 Deg.
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          5 Note
PLAT899_ALERT_4_G SHELXL97   is Deprecated and Succeeded by SHELXL       2014 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density           1 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
   7 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  28 ALERT level G = General information/check it is not something unexpected

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  11 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
  16 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

Computing details top

Data collection: CrysAlis PRO (Agilent, 2012); cell refinement: CrysAlis PRO (Agilent, 2012); data reduction: CrysAlis PRO (Agilent, 2012); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

1,3,7,9-Tetrakis[2,6-bis(1-methylethyl)phenyl]-2,2,8,8-tetraphenyl-5,10-dithia-1,3,7,9-tetraaza-2,8-disila-4,6-digermadispiro[3.1.3.1]decane acetonitrile monosolvate top

Crystal data top

C₇₂H₈₈Ge₂N₄S₂Si₂·C₂H₃N	Z = 1
M_r = 1316.00	F(000) = 694
Triclinic, P1	D_x = 1.182 Mg m⁻³
Hall symbol: -P 1	Melting point: 320 K
a = 11.0447 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.4587 (6) Å	Cell parameters from 3142 reflections
c = 13.9291 (6) Å	θ = 2.2–27.0°
α = 64.297 (4)°	µ = 0.94 mm⁻¹
β = 82.371 (4)°	T = 153 K
γ = 85.629 (4)°	Block, colorless
V = 1848.74 (14) Å³	0.15 × 0.13 × 0.11 mm

Data collection top

Agilent SuperNova Dual Source diffractometer with an Eos detector	5534 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.037
Graphite monochromator	θ_max = 25.7°, θ_min = 2.7°
ω scans	h = −13→13
Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2012)	k = −16→16
T_min = 0.871, T_max = 0.903	l = −14→16
13757 measured reflections	5839 standard reflections every 1 reflections
7010 independent reflections	intensity decay: none

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.138	H-atom parameters constrained
S = 1.08	w = 1/[σ²(F_o²) + (0.066P)² + 1.4505P] where P = (F_o² + 2F_c²)/3
7010 reflections	(Δ/σ)_max = 0.001
405 parameters	Δρ_max = 0.75 e Å⁻³
5 restraints	Δρ_min = −0.38 e Å⁻³

Special details top

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
C1	0.5999 (3)	0.8105 (3)	0.8258 (3)	0.0343 (8)
C2	0.7166 (4)	0.8406 (3)	0.8332 (3)	0.0432 (9)
C3	0.7231 (5)	0.9309 (4)	0.8568 (4)	0.0664 (13)
H3	0.7992	0.9523	0.8620	0.080*
C4	0.6212 (6)	0.9890 (4)	0.8726 (4)	0.0758 (15)
H4	0.6284	1.0488	0.8880	0.091*
C5	0.5104 (5)	0.9585 (4)	0.8656 (4)	0.0649 (13)
H5	0.4415	0.9978	0.8770	0.078*
C6	0.4960 (4)	0.8698 (3)	0.8419 (3)	0.0455 (9)
C7	0.3688 (4)	0.8415 (3)	0.8343 (3)	0.0526 (10)
H7	0.3753	0.7737	0.8239	0.063*
C8	0.3135 (5)	0.9325 (4)	0.7373 (4)	0.0771 (15)
H8A	0.3124	1.0014	0.7425	0.116*
H8B	0.2316	0.9138	0.7364	0.116*
H8C	0.3621	0.9390	0.6724	0.116*
C9	0.2836 (5)	0.8191 (5)	0.9380 (5)	0.0907 (19)
H9A	0.2061	0.7952	0.9328	0.136*
H9B	0.2721	0.8855	0.9481	0.136*
H9C	0.3195	0.7627	0.9979	0.136*
C10	0.8328 (4)	0.7778 (4)	0.8211 (3)	0.0529 (10)
H10	0.8167	0.7357	0.7819	0.063*
C11	0.8684 (5)	0.6954 (4)	0.9310 (4)	0.0730 (14)
H11A	0.8005	0.6490	0.9711	0.109*
H11B	0.8902	0.7347	0.9693	0.109*
H11C	0.9368	0.6507	0.9216	0.109*
C12	0.9418 (5)	0.8525 (5)	0.7581 (5)	0.0852 (17)
H12A	1.0091	0.8086	0.7455	0.128*
H12B	0.9655	0.8884	0.7988	0.128*
H12C	0.9187	0.9069	0.6907	0.128*
C13	0.6486 (4)	0.4640 (3)	0.7428 (3)	0.0407 (8)
C14	0.5671 (4)	0.3995 (4)	0.7257 (4)	0.0573 (11)
C15	0.6130 (6)	0.3145 (5)	0.7004 (6)	0.0928 (19)
H15	0.5597	0.2724	0.6876	0.111*
C16	0.7335 (8)	0.2918 (6)	0.6940 (7)	0.117 (3)
H16	0.7626	0.2342	0.6768	0.140*
C17	0.8142 (6)	0.3521 (5)	0.7124 (5)	0.0923 (19)
H17	0.8972	0.3347	0.7076	0.111*
C18	0.7741 (4)	0.4396 (3)	0.7384 (4)	0.0558 (11)
C19	0.4309 (5)	0.4185 (5)	0.7355 (5)	0.0757 (15)
H19	0.4156	0.4803	0.7553	0.091*
C20	0.3639 (9)	0.3199 (7)	0.8245 (8)	0.170 (5)
H20A	0.3710	0.2591	0.8054	0.254*
H20B	0.2792	0.3393	0.8342	0.254*
H20C	0.3993	0.2992	0.8901	0.254*
C21	0.3781 (7)	0.4528 (9)	0.6297 (7)	0.151 (4)
H21A	0.4010	0.3988	0.6024	0.227*
H21B	0.4095	0.5231	0.5789	0.227*
H21C	0.2907	0.4580	0.6411	0.227*
C22	0.8674 (4)	0.4998 (4)	0.7626 (4)	0.0694 (14)
H22	0.8293	0.5689	0.7602	0.083*
C23	0.9825 (6)	0.5286 (7)	0.6815 (6)	0.135 (3)
H23A	1.0348	0.4643	0.6977	0.203*
H23B	1.0252	0.5858	0.6857	0.203*
H23C	0.9596	0.5535	0.6105	0.203*
C24	0.9062 (5)	0.4330 (5)	0.8741 (5)	0.0804 (15)
H24A	0.9575	0.4766	0.8906	0.121*
H24B	0.9505	0.3679	0.8765	0.121*
H24C	0.8350	0.4121	0.9257	0.121*
C25	0.7362 (3)	0.7545 (3)	0.5812 (3)	0.0386 (8)
C26	0.7889 (4)	0.8533 (4)	0.5569 (3)	0.0545 (11)
H26	0.7620	0.8915	0.5978	0.065*
C27	0.8806 (5)	0.8973 (5)	0.4733 (4)	0.0737 (15)
H27	0.9140	0.9646	0.4584	0.088*
C28	0.9219 (5)	0.8424 (5)	0.4131 (4)	0.0829 (17)
H28	0.9851	0.8708	0.3581	0.100*
C29	0.8699 (6)	0.7446 (5)	0.4338 (4)	0.0883 (19)
H29	0.8971	0.7076	0.3918	0.106*
C30	0.7771 (5)	0.7006 (4)	0.5170 (3)	0.0645 (13)
H30	0.7420	0.6347	0.5299	0.077*
C31	0.4652 (3)	0.7543 (3)	0.6081 (3)	0.0380 (8)
C32	0.3480 (4)	0.7169 (4)	0.6525 (3)	0.0536 (10)
H32	0.3362	0.6614	0.7219	0.064*
C33	0.2480 (4)	0.7609 (4)	0.5951 (4)	0.0670 (13)
H33	0.1702	0.7349	0.6262	0.080*
C34	0.2645 (5)	0.8431 (4)	0.4920 (4)	0.0695 (14)
H34	0.1976	0.8722	0.4536	0.083*
C35	0.3779 (5)	0.8816 (4)	0.4464 (4)	0.0703 (14)
H35	0.3886	0.9373	0.3770	0.084*
C36	0.4777 (4)	0.8376 (3)	0.5037 (3)	0.0528 (10)
H36	0.5550	0.8643	0.4716	0.063*
C38	−0.0273 (16)	−0.0191 (14)	0.9955 (15)	0.128 (6)	0.50
H38A	−0.1136	−0.0196	0.9925	0.193*	0.50
H38B	0.0120	−0.0783	0.9814	0.193*	0.50
H38C	−0.0128	−0.0286	1.0654	0.193*	0.50
Ge1	0.55890 (3)	0.57094 (3)	0.88889 (3)	0.03020 (13)
N1	0.5904 (3)	0.7178 (2)	0.8016 (2)	0.0311 (6)
N2	0.6031 (3)	0.5576 (2)	0.7626 (2)	0.0343 (6)
N3	0.1041 (12)	0.1467 (8)	0.8636 (8)	0.114 (4)	0.50
S1	0.36302 (8)	0.52913 (8)	0.95938 (7)	0.0412 (2)
Si1	0.60204 (9)	0.69914 (7)	0.68380 (7)	0.0309 (2)
C37	0.0482 (11)	0.0770 (9)	0.9190 (9)	0.158 (9)	0.50

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.045 (2)	0.0297 (17)	0.0255 (16)	−0.0063 (15)	−0.0003 (14)	−0.0094 (13)
C2	0.051 (2)	0.044 (2)	0.0345 (19)	−0.0137 (17)	−0.0031 (17)	−0.0147 (16)
C3	0.081 (4)	0.063 (3)	0.067 (3)	−0.026 (3)	−0.012 (3)	−0.033 (2)
C4	0.106 (5)	0.057 (3)	0.081 (4)	−0.011 (3)	−0.008 (3)	−0.046 (3)
C5	0.087 (4)	0.048 (3)	0.067 (3)	0.003 (2)	0.000 (3)	−0.034 (2)
C6	0.058 (3)	0.037 (2)	0.0371 (19)	−0.0023 (17)	0.0035 (17)	−0.0134 (16)
C7	0.046 (3)	0.041 (2)	0.062 (3)	0.0037 (18)	0.0064 (19)	−0.0183 (19)
C8	0.066 (4)	0.063 (3)	0.091 (4)	0.009 (3)	−0.019 (3)	−0.021 (3)
C9	0.079 (4)	0.081 (4)	0.092 (4)	−0.005 (3)	0.036 (3)	−0.030 (3)
C10	0.045 (2)	0.066 (3)	0.052 (2)	−0.016 (2)	−0.0043 (19)	−0.027 (2)
C11	0.066 (3)	0.071 (3)	0.080 (3)	0.000 (3)	−0.024 (3)	−0.026 (3)
C12	0.058 (3)	0.113 (5)	0.085 (4)	−0.036 (3)	0.006 (3)	−0.041 (3)
C13	0.050 (2)	0.0343 (19)	0.0366 (19)	−0.0032 (16)	0.0024 (16)	−0.0155 (15)
C14	0.066 (3)	0.052 (2)	0.063 (3)	−0.009 (2)	0.000 (2)	−0.035 (2)
C15	0.104 (5)	0.081 (4)	0.130 (5)	0.001 (3)	−0.014 (4)	−0.078 (4)
C16	0.124 (7)	0.102 (5)	0.170 (8)	0.028 (5)	−0.019 (5)	−0.105 (6)
C17	0.073 (4)	0.089 (4)	0.126 (5)	0.025 (3)	−0.004 (4)	−0.063 (4)
C18	0.050 (3)	0.048 (2)	0.065 (3)	0.0047 (19)	0.001 (2)	−0.023 (2)
C19	0.065 (3)	0.091 (4)	0.098 (4)	−0.026 (3)	0.003 (3)	−0.065 (3)
C20	0.151 (8)	0.147 (7)	0.220 (11)	−0.093 (6)	0.100 (8)	−0.107 (8)
C21	0.083 (5)	0.271 (11)	0.178 (8)	0.031 (6)	−0.054 (5)	−0.162 (9)
C22	0.041 (3)	0.057 (3)	0.097 (4)	0.002 (2)	−0.007 (2)	−0.021 (3)
C23	0.058 (4)	0.160 (7)	0.119 (6)	−0.027 (4)	0.002 (4)	0.005 (5)
C24	0.060 (3)	0.090 (4)	0.093 (4)	0.004 (3)	−0.009 (3)	−0.041 (3)
C25	0.037 (2)	0.042 (2)	0.0282 (17)	−0.0048 (15)	0.0030 (14)	−0.0084 (15)
C26	0.056 (3)	0.062 (3)	0.040 (2)	−0.023 (2)	0.0070 (19)	−0.0171 (19)
C27	0.064 (3)	0.091 (4)	0.052 (3)	−0.044 (3)	0.007 (2)	−0.015 (3)
C28	0.053 (3)	0.112 (5)	0.050 (3)	−0.017 (3)	0.020 (2)	−0.008 (3)
C29	0.097 (5)	0.101 (4)	0.051 (3)	0.011 (4)	0.028 (3)	−0.030 (3)
C30	0.080 (4)	0.060 (3)	0.047 (2)	−0.011 (2)	0.020 (2)	−0.023 (2)
C31	0.040 (2)	0.0387 (19)	0.0339 (18)	−0.0034 (15)	−0.0050 (15)	−0.0139 (15)
C32	0.042 (2)	0.059 (3)	0.050 (2)	−0.0059 (19)	−0.0017 (19)	−0.015 (2)
C33	0.037 (3)	0.079 (3)	0.085 (4)	−0.005 (2)	−0.009 (2)	−0.034 (3)
C34	0.059 (3)	0.086 (4)	0.070 (3)	0.012 (3)	−0.032 (3)	−0.034 (3)
C35	0.070 (4)	0.078 (3)	0.046 (3)	0.008 (3)	−0.019 (2)	−0.009 (2)
C36	0.048 (3)	0.061 (3)	0.038 (2)	−0.004 (2)	−0.0073 (18)	−0.0090 (19)
C38	0.085 (13)	0.118 (15)	0.194 (19)	−0.046 (10)	−0.002 (13)	−0.074 (13)
Ge1	0.0324 (2)	0.0288 (2)	0.02414 (18)	−0.00556 (14)	0.00189 (13)	−0.00704 (14)
N1	0.0337 (16)	0.0311 (14)	0.0255 (13)	−0.0047 (11)	0.0001 (11)	−0.0096 (11)
N2	0.0418 (18)	0.0314 (15)	0.0276 (14)	−0.0092 (12)	0.0045 (12)	−0.0116 (12)
N3	0.185 (14)	0.074 (7)	0.072 (7)	−0.027 (8)	0.007 (7)	−0.023 (5)
S1	0.0318 (5)	0.0476 (5)	0.0295 (4)	−0.0063 (4)	−0.0011 (4)	−0.0027 (4)
Si1	0.0323 (5)	0.0330 (5)	0.0241 (4)	−0.0062 (4)	0.0015 (4)	−0.0094 (4)
C37	0.20 (2)	0.103 (16)	0.16 (2)	−0.043 (15)	0.008 (18)	−0.046 (14)

Geometric parameters (Å, º) top

C1—C6	1.397 (5)	C21—H21C	0.9600
C1—C2	1.410 (5)	C22—C24	1.520 (7)
C1—N1	1.441 (4)	C22—C23	1.535 (8)
C2—C3	1.399 (6)	C22—H22	0.9800
C2—C10	1.513 (6)	C23—H23A	0.9600
C3—C4	1.368 (7)	C23—H23B	0.9600
C3—H3	0.9300	C23—H23C	0.9600
C4—C5	1.349 (7)	C24—H24A	0.9600
C4—H4	0.9300	C24—H24B	0.9600
C5—C6	1.395 (6)	C24—H24C	0.9600
C5—H5	0.9300	C25—C26	1.377 (5)
C6—C7	1.511 (6)	C25—C30	1.391 (5)
C7—C9	1.539 (6)	C25—Si1	1.864 (4)
C7—C8	1.539 (6)	C26—C27	1.383 (6)
C7—H7	0.9800	C26—H26	0.9300
C8—H8A	0.9600	C27—C28	1.358 (8)
C8—H8B	0.9600	C27—H27	0.9300
C8—H8C	0.9600	C28—C29	1.374 (8)
C9—H9A	0.9600	C28—H28	0.9300
C9—H9B	0.9600	C29—C30	1.388 (7)
C9—H9C	0.9600	C29—H29	0.9300
C10—C11	1.533 (6)	C30—H30	0.9300
C10—C12	1.538 (6)	C31—C32	1.388 (6)
C10—H10	0.9800	C31—C36	1.395 (5)
C11—H11A	0.9600	C31—Si1	1.877 (4)
C11—H11B	0.9600	C32—C33	1.391 (6)
C11—H11C	0.9600	C32—H32	0.9300
C12—H12A	0.9600	C33—C34	1.379 (7)
C12—H12B	0.9600	C33—H33	0.9300
C12—H12C	0.9600	C34—C35	1.357 (7)
C13—C18	1.400 (6)	C34—H34	0.9300
C13—C14	1.405 (6)	C35—C36	1.388 (6)
C13—N2	1.444 (4)	C35—H35	0.9300
C14—C15	1.380 (6)	C36—H36	0.9300
C14—C19	1.505 (7)	C38—C38ⁱ	0.88 (3)
C15—C16	1.343 (9)	C38—C37ⁱ	1.11 (3)
C15—H15	0.9300	C38—C37	1.495 (9)
C16—C17	1.367 (9)	C38—H38A	0.9600
C16—H16	0.9300	C38—H38B	0.9599
C17—C18	1.400 (7)	C38—H38C	0.9600
C17—H17	0.9300	Ge1—N2	1.843 (3)
C18—C22	1.514 (7)	Ge1—N1	1.847 (3)
C19—C21	1.524 (9)	Ge1—S1ⁱⁱ	2.2050 (9)
C19—C20	1.525 (9)	Ge1—S1	2.2590 (10)
C19—H19	0.9800	Ge1—Si1	2.6179 (9)
C20—H20A	0.9600	N1—Si1	1.752 (3)
C20—H20B	0.9600	N2—Si1	1.738 (3)
C20—H20C	0.9600	N3—C37	1.091 (9)
C21—H21A	0.9600	S1—Ge1ⁱⁱ	2.2050 (9)
C21—H21B	0.9600	C37—C38ⁱ	1.11 (3)

C6—C1—C2	120.3 (3)	C23—C22—H22	107.9
C6—C1—N1	121.0 (3)	C22—C23—H23A	109.5
C2—C1—N1	118.7 (3)	C22—C23—H23B	109.5
C3—C2—C1	117.5 (4)	H23A—C23—H23B	109.5
C3—C2—C10	119.2 (4)	C22—C23—H23C	109.5
C1—C2—C10	123.3 (3)	H23A—C23—H23C	109.5
C4—C3—C2	122.3 (5)	H23B—C23—H23C	109.5
C4—C3—H3	118.9	C22—C24—H24A	109.5
C2—C3—H3	118.9	C22—C24—H24B	109.5
C5—C4—C3	119.3 (4)	H24A—C24—H24B	109.5
C5—C4—H4	120.3	C22—C24—H24C	109.5
C3—C4—H4	120.3	H24A—C24—H24C	109.5
C4—C5—C6	122.1 (5)	H24B—C24—H24C	109.5
C4—C5—H5	119.0	C26—C25—C30	117.4 (4)
C6—C5—H5	119.0	C26—C25—Si1	123.3 (3)
C5—C6—C1	118.6 (4)	C30—C25—Si1	118.8 (3)
C5—C6—C7	118.9 (4)	C25—C26—C27	121.9 (4)
C1—C6—C7	122.5 (3)	C25—C26—H26	119.0
C6—C7—C9	111.8 (4)	C27—C26—H26	119.0
C6—C7—C8	111.4 (4)	C28—C27—C26	120.0 (5)
C9—C7—C8	110.4 (4)	C28—C27—H27	120.0
C6—C7—H7	107.7	C26—C27—H27	120.0
C9—C7—H7	107.7	C27—C28—C29	119.7 (4)
C8—C7—H7	107.7	C27—C28—H28	120.2
C7—C8—H8A	109.5	C29—C28—H28	120.2
C7—C8—H8B	109.5	C28—C29—C30	120.5 (5)
H8A—C8—H8B	109.5	C28—C29—H29	119.7
C7—C8—H8C	109.5	C30—C29—H29	119.7
H8A—C8—H8C	109.5	C29—C30—C25	120.4 (5)
H8B—C8—H8C	109.5	C29—C30—H30	119.8
C7—C9—H9A	109.5	C25—C30—H30	119.8
C7—C9—H9B	109.5	C32—C31—C36	117.0 (4)
H9A—C9—H9B	109.5	C32—C31—Si1	122.5 (3)
C7—C9—H9C	109.5	C36—C31—Si1	120.4 (3)
H9A—C9—H9C	109.5	C31—C32—C33	121.2 (4)
H9B—C9—H9C	109.5	C31—C32—H32	119.4
C2—C10—C11	110.7 (4)	C33—C32—H32	119.4
C2—C10—C12	113.7 (4)	C34—C33—C32	119.9 (4)
C11—C10—C12	109.0 (4)	C34—C33—H33	120.0
C2—C10—H10	107.7	C32—C33—H33	120.0
C11—C10—H10	107.7	C35—C34—C33	120.3 (4)
C12—C10—H10	107.7	C35—C34—H34	119.9
C10—C11—H11A	109.5	C33—C34—H34	119.9
C10—C11—H11B	109.5	C34—C35—C36	119.8 (4)
H11A—C11—H11B	109.5	C34—C35—H35	120.1
C10—C11—H11C	109.5	C36—C35—H35	120.1
H11A—C11—H11C	109.5	C35—C36—C31	121.8 (4)
H11B—C11—H11C	109.5	C35—C36—H36	119.1
C10—C12—H12A	109.5	C31—C36—H36	119.1
C10—C12—H12B	109.5	C38ⁱ—C38—C37ⁱ	97 (3)
H12A—C12—H12B	109.5	C38ⁱ—C38—C37	47 (2)
C10—C12—H12C	109.5	C37ⁱ—C38—C37	144.4 (16)
H12A—C12—H12C	109.5	C38ⁱ—C38—H38A	140.5
H12B—C12—H12C	109.5	C37ⁱ—C38—H38A	85.0
C18—C13—C14	120.5 (4)	C37—C38—H38A	121.2
C18—C13—N2	119.6 (3)	C38ⁱ—C38—H38B	110.0
C14—C13—N2	119.9 (4)	C37ⁱ—C38—H38B	89.8
C15—C14—C13	119.1 (5)	C37—C38—H38B	101.7
C15—C14—C19	118.5 (5)	H38A—C38—H38B	109.5
C13—C14—C19	122.4 (4)	C38ⁱ—C38—H38C	58.0
C16—C15—C14	120.9 (6)	C37ⁱ—C38—H38C	39.9
C16—C15—H15	119.6	C37—C38—H38C	104.9
C14—C15—H15	119.6	H38A—C38—H38C	109.5
C15—C16—C17	121.0 (5)	H38B—C38—H38C	109.5
C15—C16—H16	119.5	N2—Ge1—N1	82.41 (12)
C17—C16—H16	119.5	N2—Ge1—S1ⁱⁱ	124.77 (9)
C16—C17—C18	121.2 (6)	N1—Ge1—S1ⁱⁱ	125.33 (9)
C16—C17—H17	119.4	N2—Ge1—S1	114.90 (10)
C18—C17—H17	119.4	N1—Ge1—S1	116.58 (9)
C13—C18—C17	117.3 (5)	S1ⁱⁱ—Ge1—S1	94.97 (3)
C13—C18—C22	124.1 (4)	N2—Ge1—Si1	41.47 (9)
C17—C18—C22	118.6 (5)	N1—Ge1—Si1	41.92 (8)
C14—C19—C21	112.4 (5)	S1ⁱⁱ—Ge1—Si1	146.78 (4)
C14—C19—C20	112.5 (6)	S1—Ge1—Si1	118.22 (3)
C21—C19—C20	110.9 (6)	C1—N1—Si1	135.0 (2)
C14—C19—H19	106.8	C1—N1—Ge1	131.7 (2)
C21—C19—H19	106.8	Si1—N1—Ge1	93.30 (12)
C20—C19—H19	106.8	C13—N2—Si1	133.6 (2)
C19—C20—H20A	109.5	C13—N2—Ge1	131.2 (2)
C19—C20—H20B	109.5	Si1—N2—Ge1	93.92 (13)
H20A—C20—H20B	109.5	Ge1ⁱⁱ—S1—Ge1	85.03 (3)
C19—C20—H20C	109.5	N2—Si1—N1	88.31 (13)
H20A—C20—H20C	109.5	N2—Si1—C25	116.31 (15)
H20B—C20—H20C	109.5	N1—Si1—C25	119.45 (15)
C19—C21—H21A	109.5	N2—Si1—C31	114.79 (15)
C19—C21—H21B	109.5	N1—Si1—C31	113.02 (15)
H21A—C21—H21B	109.5	C25—Si1—C31	104.96 (16)
C19—C21—H21C	109.5	N2—Si1—Ge1	44.61 (9)
H21A—C21—H21C	109.5	N1—Si1—Ge1	44.78 (9)
H21B—C21—H21C	109.5	C25—Si1—Ge1	138.43 (12)
C18—C22—C24	111.4 (4)	C31—Si1—Ge1	116.59 (12)
C18—C22—C23	113.1 (5)	N3—C37—C38ⁱ	144.0 (16)
C24—C22—C23	108.3 (5)	N3—C37—C38	179.4 (4)
C18—C22—H22	107.9	C38ⁱ—C37—C38	35.6 (16)
C24—C22—H22	107.9

C6—C1—C2—C3	0.0 (5)	Si1—Ge1—N1—C1	179.5 (4)
N1—C1—C2—C3	180.0 (3)	N2—Ge1—N1—Si1	10.54 (13)
C6—C1—C2—C10	177.6 (3)	S1ⁱⁱ—Ge1—N1—Si1	138.19 (8)
N1—C1—C2—C10	−2.3 (5)	S1—Ge1—N1—Si1	−103.55 (10)
C1—C2—C3—C4	0.1 (7)	C18—C13—N2—Si1	76.5 (5)
C10—C2—C3—C4	−177.7 (4)	C14—C13—N2—Si1	−102.1 (4)
C2—C3—C4—C5	0.2 (8)	C18—C13—N2—Ge1	−86.7 (4)
C3—C4—C5—C6	−0.5 (8)	C14—C13—N2—Ge1	94.7 (4)
C4—C5—C6—C1	0.6 (7)	N1—Ge1—N2—C13	157.2 (3)
C4—C5—C6—C7	−179.4 (4)	S1ⁱⁱ—Ge1—N2—C13	29.1 (4)
C2—C1—C6—C5	−0.3 (5)	S1—Ge1—N2—C13	−87.0 (3)
N1—C1—C6—C5	179.7 (3)	Si1—Ge1—N2—C13	167.9 (4)
C2—C1—C6—C7	179.7 (3)	N1—Ge1—N2—Si1	−10.64 (13)
N1—C1—C6—C7	−0.4 (5)	S1ⁱⁱ—Ge1—N2—Si1	−138.79 (8)
C5—C6—C7—C9	−56.7 (5)	S1—Ge1—N2—Si1	105.20 (11)
C1—C6—C7—C9	123.4 (4)	N2—Ge1—S1—Ge1ⁱⁱ	132.18 (10)
C5—C6—C7—C8	67.3 (5)	N1—Ge1—S1—Ge1ⁱⁱ	−133.84 (9)
C1—C6—C7—C8	−112.7 (4)	S1ⁱⁱ—Ge1—S1—Ge1ⁱⁱ	0.0
C3—C2—C10—C11	81.3 (5)	Si1—Ge1—S1—Ge1ⁱⁱ	178.67 (3)
C1—C2—C10—C11	−96.3 (4)	C13—N2—Si1—N1	−156.2 (3)
C3—C2—C10—C12	−41.8 (5)	Ge1—N2—Si1—N1	11.13 (13)
C1—C2—C10—C12	140.6 (4)	C13—N2—Si1—C25	−34.0 (4)
C18—C13—C14—C15	−2.5 (7)	Ge1—N2—Si1—C25	133.41 (15)
N2—C13—C14—C15	176.1 (4)	C13—N2—Si1—C31	89.1 (4)
C18—C13—C14—C19	176.5 (5)	Ge1—N2—Si1—C31	−103.53 (16)
N2—C13—C14—C19	−4.8 (6)	C13—N2—Si1—Ge1	−167.4 (4)
C13—C14—C15—C16	1.2 (10)	C1—N1—Si1—N2	169.4 (3)
C19—C14—C15—C16	−177.9 (7)	Ge1—N1—Si1—N2	−11.09 (13)
C14—C15—C16—C17	0.1 (12)	C1—N1—Si1—C25	49.9 (4)
C15—C16—C17—C18	−0.1 (12)	Ge1—N1—Si1—C25	−130.60 (15)
C14—C13—C18—C17	2.4 (7)	C1—N1—Si1—C31	−74.3 (4)
N2—C13—C18—C17	−176.2 (4)	Ge1—N1—Si1—C31	105.21 (15)
C14—C13—C18—C22	−175.9 (4)	C1—N1—Si1—Ge1	−179.5 (4)
N2—C13—C18—C22	5.4 (6)	C26—C25—Si1—N2	−141.4 (3)
C16—C17—C18—C13	−1.2 (9)	C30—C25—Si1—N2	46.3 (4)
C16—C17—C18—C22	177.3 (6)	C26—C25—Si1—N1	−37.4 (4)
C15—C14—C19—C21	−64.4 (8)	C30—C25—Si1—N1	150.2 (3)
C13—C14—C19—C21	116.5 (6)	C26—C25—Si1—C31	90.6 (4)
C15—C14—C19—C20	61.7 (7)	C30—C25—Si1—C31	−81.8 (4)
C13—C14—C19—C20	−117.4 (6)	C26—C25—Si1—Ge1	−91.1 (4)
C13—C18—C22—C24	101.9 (5)	C30—C25—Si1—Ge1	96.5 (3)
C17—C18—C22—C24	−76.4 (6)	C32—C31—Si1—N2	40.0 (4)
C13—C18—C22—C23	−135.8 (5)	C36—C31—Si1—N2	−141.3 (3)
C17—C18—C22—C23	45.9 (7)	C32—C31—Si1—N1	−59.3 (4)
C30—C25—C26—C27	−1.2 (7)	C36—C31—Si1—N1	119.4 (3)
Si1—C25—C26—C27	−173.6 (4)	C32—C31—Si1—C25	168.9 (3)
C25—C26—C27—C28	−0.6 (8)	C36—C31—Si1—C25	−12.4 (4)
C26—C27—C28—C29	1.8 (9)	C32—C31—Si1—Ge1	−9.8 (4)
C27—C28—C29—C30	−1.2 (9)	C36—C31—Si1—Ge1	168.9 (3)
C28—C29—C30—C25	−0.6 (9)	N1—Ge1—Si1—N2	164.10 (19)
C26—C25—C30—C29	1.7 (7)	S1ⁱⁱ—Ge1—Si1—N2	81.03 (15)
Si1—C25—C30—C29	174.5 (4)	S1—Ge1—Si1—N2	−96.56 (15)
C36—C31—C32—C33	−0.1 (6)	N2—Ge1—Si1—N1	−164.10 (19)
Si1—C31—C32—C33	178.7 (3)	S1ⁱⁱ—Ge1—Si1—N1	−83.07 (14)
C31—C32—C33—C34	0.1 (7)	S1—Ge1—Si1—N1	99.34 (13)
C32—C33—C34—C35	−0.3 (8)	N2—Ge1—Si1—C25	−78.9 (2)
C33—C34—C35—C36	0.3 (8)	N1—Ge1—Si1—C25	85.2 (2)
C34—C35—C36—C31	−0.3 (8)	S1ⁱⁱ—Ge1—Si1—C25	2.1 (2)
C32—C31—C36—C35	0.1 (6)	S1—Ge1—Si1—C25	−175.49 (18)
Si1—C31—C36—C35	−178.7 (4)	N2—Ge1—Si1—C31	99.21 (19)
C6—C1—N1—Si1	95.0 (4)	N1—Ge1—Si1—C31	−96.68 (18)
C2—C1—N1—Si1	−85.0 (4)	S1ⁱⁱ—Ge1—Si1—C31	−179.76 (13)
C6—C1—N1—Ge1	−84.3 (4)	S1—Ge1—Si1—C31	2.66 (14)
C2—C1—N1—Ge1	95.7 (4)	C38ⁱ—C38—C37—N3	45 (39)
N2—Ge1—N1—C1	−170.0 (3)	C37ⁱ—C38—C37—N3	45 (39)
S1ⁱⁱ—Ge1—N1—C1	−42.3 (3)	C37ⁱ—C38—C37—C38ⁱ	0.000 (8)
S1—Ge1—N1—C1	76.0 (3)

Symmetry codes: (i) −x, −y, −z+2; (ii) −x+1, −y+1, −z+2.

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1,3,7,9-Tetra­kis[2,6-bis­(1-methyl­eth­yl)phen­yl]-2,2,8,8-tetra­phen­yl-5,10-di­thia-1,3,7,9-tetra­aza-2,8-disila-4,6-digermadi­spiro­[3.1.3.1]decane aceto­nitrile monosolvate

Supporting information

Key indicators

checkCIF/PLATON results

1,3,7,9-Tetrakis[2,6-bis(1-methylethyl)phenyl]-2,2,8,8-tetraphenyl-5,10-dithia-1,3,7,9-tetraaza-2,8-disila-4,6-digermadispiro[3.1.3.1]decane acetonitrile monosolvate