3182

Table 1 Crystal data and structure refinement for 3182.
Identification code	3182
Empirical formula	C₂₈H₆₈Li₄O₈Si₄
Formula weight	672.94
Temperature/K	173.15
Crystal system	monoclinic
Space group	P2₁/c
a/Å	20.3421(14)
b/Å	10.7413(5)
c/Å	21.0670(16)
α/°	90
β/°	112.664(9)
γ/°	90
Volume/Å³	4247.7(5)
Z	4
ρ_calcg/cm³	1.052
μ/mm^‑1	0.176
F(000)	1472.0
Crystal size/mm³	0.3 × 0.23 × 0.21
Radiation	MoKα (λ = 0.71073)
2Θ range for data collection/°	4.19 to 50
Index ranges	-24 ≤ h ≤ 24, -12 ≤ k ≤ 12, -25 ≤ l ≤ 24
Reflections collected	46058
Independent reflections	7469 [R_int = 0.0673, R_sigma = 0.0436]
Data/restraints/parameters	7469/0/409
Goodness-of-fit on F²	1.134
Final R indexes [I>=2σ (I)]	R₁ = 0.0710, wR₂ = 0.1920
Final R indexes [all data]	R₁ = 0.0931, wR₂ = 0.2057
Largest diff. peak/hole / e Å^-3	0.43/-0.33

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for 3182. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.
Atom	x	y	z	U(eq)
Si3	11247.9(6)	11341.2(10)	1251.2(6)	38.9(3)
Si1	13955.3(5)	11197.5(9)	3555.2(5)	29.1(3)
Si4	13114.7(6)	7435.0(11)	1759.3(6)	40.7(3)
Si2	11590.5(6)	8726.2(11)	3504.9(6)	40.9(3)
O1	13230.9(12)	10562(2)	3054.8(12)	28.7(6)
O4	12790.2(12)	8379(2)	2141.1(12)	29.4(6)
O2	12010.6(13)	9068(2)	3027.7(12)	33.4(6)
O3	11875.7(12)	10591(2)	1825.4(12)	32.4(6)
O5	13587.3(15)	7578(3)	3815.9(13)	42.9(7)
O7	13394.5(15)	11062(3)	1557.8(15)	46.6(7)
O6	11867.5(15)	12274(3)	3145.1(17)	54.6(8)
O8	11064.2(15)	7714(3)	1443.5(15)	49.9(8)
C2	13965(2)	11391(4)	4450(2)	44.7(10)
C9	10352(2)	10930(5)	1252(2)	51.8(11)
C1	14757(2)	10240(4)	3641(2)	43.3(10)
C13	13512(3)	6261(4)	3691(2)	54.3(12)
C3	14093(2)	12777(4)	3245(2)	43.8(10)
C16	13929(2)	7795(4)	4539(2)	47.5(11)
C15	14241(3)	6554(5)	4853(2)	60.5(13)
C21	13161(3)	12290(4)	1295(2)	53.8(12)
C7	11219(3)	11023(5)	363(2)	57.7(13)
C26	10567(3)	6453(5)	466(3)	61.7(14)
C28	10734(3)	6663(5)	1614(3)	58.8(13)
C14	13735(3)	5652(5)	4388(3)	66.9(15)
C6	11920(3)	9654(5)	4331(2)	62.5(13)
C23	14164(3)	11771(5)	1049(3)	67.1(15)
C27	10218(2)	6151(4)	941(3)	59.5(13)
C24	14078(3)	10829(5)	1537(3)	59.3(13)
C11	14112(2)	7337(5)	2204(3)	63.9(14)
C12	12917(3)	7919(6)	846(2)	68.4(15)
C20	12292(3)	13326(5)	3489(3)	63.5(14)
C8	11341(3)	13077(4)	1383(3)	66.8(15)
C22	13777(3)	12871(5)	1171(3)	67.4(15)
C4	11697(3)	7038(5)	3757(3)	61.6(13)
C5	10605(2)	9002(5)	3059(3)	59.4(13)
C19	11993(3)	13668(6)	4011(3)	72.9(16)
C10	12754(3)	5811(4)	1707(3)	67.1(15)
C25	10897(3)	7718(5)	715(2)	60.5(13)
C18	11202(3)	13495(7)	3602(4)	88(2)
C17	11156(3)	12523(6)	3108(3)	72.2(16)
Li4	11838(3)	8820(6)	2060(3)	33.3(14)
Li3	12876(3)	10199(6)	2070(3)	31.0(13)
Li2	12216(3)	10782(6)	2824(3)	31.5(13)
Li1	12990(3)	8805(6)	3095(3)	31.1(13)

Table 2 Fractional Atomic Coordinates (×10⁴) and Equivalent Isotropic Displacement Parameters (Å²×10³) for 3182. U_eq is defined as 1/3 of of the trace of the orthogonalised U_IJ tensor.

Atom

U(eq)

Si3

11247.9(6)

11341.2(10)

1251.2(6)

38.9(3)

Si1

13955.3(5)

11197.5(9)

3555.2(5)

29.1(3)

Si4

13114.7(6)

7435.0(11)

1759.3(6)

40.7(3)

Si2

11590.5(6)

8726.2(11)

3504.9(6)

40.9(3)

13230.9(12)

10562(2)

3054.8(12)

28.7(6)

12790.2(12)

8379(2)

2141.1(12)

29.4(6)

12010.6(13)

9068(2)

3027.7(12)

33.4(6)

11875.7(12)

10591(2)

1825.4(12)

32.4(6)

13587.3(15)

7578(3)

3815.9(13)

42.9(7)

13394.5(15)

11062(3)

1557.8(15)

46.6(7)

11867.5(15)

12274(3)

3145.1(17)

54.6(8)

11064.2(15)

7714(3)

1443.5(15)

49.9(8)

13965(2)

11391(4)

4450(2)

44.7(10)

10352(2)

10930(5)

1252(2)

51.8(11)

14757(2)

10240(4)

3641(2)

43.3(10)

C13

13512(3)

6261(4)

3691(2)

54.3(12)

14093(2)

12777(4)

3245(2)

43.8(10)

C16

13929(2)

7795(4)

4539(2)

47.5(11)

C15

14241(3)

6554(5)

4853(2)

60.5(13)

C21

13161(3)

12290(4)

1295(2)

53.8(12)

11219(3)

11023(5)

363(2)

57.7(13)

C26

10567(3)

6453(5)

466(3)

61.7(14)

C28

10734(3)

6663(5)

1614(3)

58.8(13)

C14

13735(3)

5652(5)

4388(3)

66.9(15)

11920(3)

9654(5)

4331(2)

62.5(13)

C23

14164(3)

11771(5)

1049(3)

67.1(15)

C27

10218(2)

6151(4)

941(3)

59.5(13)

C24

14078(3)

10829(5)

1537(3)

59.3(13)

C11

14112(2)

7337(5)

2204(3)

63.9(14)

C12

12917(3)

7919(6)

846(2)

68.4(15)

C20

12292(3)

13326(5)

3489(3)

63.5(14)

11341(3)

13077(4)

1383(3)

66.8(15)

C22

13777(3)

12871(5)

1171(3)

67.4(15)

11697(3)

7038(5)

3757(3)

61.6(13)

10605(2)

9002(5)

3059(3)

59.4(13)

C19

11993(3)

13668(6)

4011(3)

72.9(16)

C10

12754(3)

5811(4)

1707(3)

67.1(15)

C25

10897(3)

7718(5)

715(2)

60.5(13)

C18

11202(3)

13495(7)

3602(4)

88(2)

C17

11156(3)

12523(6)

3108(3)

72.2(16)

Li4

11838(3)

8820(6)

2060(3)

33.3(14)

Li3

12876(3)

10199(6)

2070(3)

31.0(13)

Li2

12216(3)

10782(6)

2824(3)

31.5(13)

Li1

12990(3)

8805(6)

3095(3)

31.1(13)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for 3182. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].
Atom	U₁₁	U₂₂	U₃₃	U₂₃	U₁₃	U₁₂
Si3	29.6(6)	38.1(6)	36.3(6)	6.3(5)	-1.5(5)	1.0(5)
Si1	22.4(5)	35.2(5)	23.9(5)	-4.4(4)	2.4(4)	-3.3(4)
Si4	39.4(6)	40.2(6)	42.7(7)	-12.9(5)	16.3(5)	-0.5(5)
Si2	34.4(6)	51.5(7)	38.4(6)	2.3(5)	15.8(5)	-3.2(5)
O1	22.6(12)	33.0(13)	23.1(12)	-4.9(10)	0.8(10)	-1.9(10)
O4	29.8(13)	29.0(13)	26.1(13)	-2(1)	7.2(11)	-0.5(10)
O2	27.4(13)	40.7(15)	30.3(14)	1.2(11)	9.1(11)	-2.1(11)
O3	27.9(13)	32.9(13)	27.5(13)	-0.4(11)	0.9(11)	0.4(11)
O5	44.2(16)	41.7(16)	29.8(14)	7.9(12)	0.0(12)	2.9(13)
O7	49.1(17)	50.7(17)	46.7(17)	2.3(14)	25.7(14)	-11.7(14)
O6	36.2(16)	55.1(19)	69(2)	-26.0(16)	16.5(15)	5.4(14)
O8	46.4(17)	46.8(17)	39.1(17)	-3.8(13)	-2.9(13)	-16.1(14)
C2	46(2)	54(3)	26(2)	-8.0(18)	4.6(18)	-4(2)
C9	32(2)	62(3)	49(3)	-1(2)	2(2)	-1(2)
C1	31(2)	51(2)	43(2)	5(2)	8.2(18)	4.2(18)
C13	62(3)	42(2)	46(3)	-1(2)	7(2)	-5(2)
C3	41(2)	39(2)	45(2)	-4.5(19)	8.6(19)	-5.9(18)
C16	51(3)	48(3)	34(2)	2.1(19)	7(2)	-4(2)
C15	55(3)	70(3)	42(3)	21(2)	3(2)	0(2)
C21	55(3)	53(3)	50(3)	9(2)	16(2)	-8(2)
C7	49(3)	74(3)	36(2)	10(2)	1(2)	-5(2)
C26	66(3)	54(3)	45(3)	-13(2)	0(2)	0(2)
C28	62(3)	57(3)	61(3)	-14(2)	27(3)	-22(2)
C14	73(3)	50(3)	59(3)	14(2)	4(3)	1(3)
C6	69(3)	76(3)	47(3)	-4(3)	26(3)	-1(3)
C23	70(3)	84(4)	57(3)	6(3)	35(3)	-17(3)
C27	40(2)	46(3)	79(4)	-17(2)	8(2)	-14(2)
C24	55(3)	69(3)	58(3)	4(3)	27(3)	-4(2)
C11	43(3)	71(3)	78(4)	-6(3)	25(3)	14(2)
C12	77(4)	92(4)	40(3)	-22(3)	27(3)	-18(3)
C20	48(3)	59(3)	82(4)	-19(3)	24(3)	-2(2)
C8	57(3)	41(3)	78(4)	13(2)	-1(3)	4(2)
C22	85(4)	61(3)	67(3)	11(3)	40(3)	-18(3)
C4	59(3)	63(3)	66(3)	14(3)	27(3)	-2(2)
C5	39(2)	70(3)	69(3)	-3(3)	21(2)	-2(2)
C19	70(4)	70(4)	73(4)	-30(3)	21(3)	-3(3)
C10	71(3)	40(3)	85(4)	-23(3)	25(3)	-3(2)
C25	59(3)	68(3)	42(3)	1(2)	6(2)	-10(3)
C18	55(3)	102(5)	110(5)	-56(4)	35(3)	-15(3)
C17	40(3)	80(4)	91(4)	-26(3)	20(3)	8(3)
Li4	27(3)	34(3)	29(3)	0(3)	0(3)	-4(3)
Li3	29(3)	38(3)	22(3)	-1(2)	6(2)	-3(3)
Li2	29(3)	32(3)	33(3)	-5(3)	12(3)	5(3)
Li1	28(3)	32(3)	29(3)	-3(3)	6(3)	-2(2)

Table 3 Anisotropic Displacement Parameters (Å²×10³) for 3182. The Anisotropic displacement factor exponent takes the form: -2π²[h²a*²U₁₁+2hka*b*U₁₂+…].

Atom

U₁₁

U₂₂

U₃₃

U₂₃

U₁₃

U₁₂

Si3

29.6(6)

38.1(6)

36.3(6)

6.3(5)

-1.5(5)

1.0(5)

Si1

22.4(5)

35.2(5)

23.9(5)

-4.4(4)

2.4(4)

-3.3(4)

Si4

39.4(6)

40.2(6)

42.7(7)

-12.9(5)

16.3(5)

-0.5(5)

Si2

34.4(6)

51.5(7)

38.4(6)

2.3(5)

15.8(5)

-3.2(5)

22.6(12)

33.0(13)

23.1(12)

-4.9(10)

0.8(10)

-1.9(10)

29.8(13)

29.0(13)

26.1(13)

-2(1)

7.2(11)

-0.5(10)

27.4(13)

40.7(15)

30.3(14)

1.2(11)

9.1(11)

-2.1(11)

27.9(13)

32.9(13)

27.5(13)

-0.4(11)

0.9(11)

0.4(11)

44.2(16)

41.7(16)

29.8(14)

7.9(12)

0.0(12)

2.9(13)

49.1(17)

50.7(17)

46.7(17)

2.3(14)

25.7(14)

-11.7(14)

36.2(16)

55.1(19)

69(2)

-26.0(16)

16.5(15)

5.4(14)

46.4(17)

46.8(17)

39.1(17)

-3.8(13)

-2.9(13)

-16.1(14)

46(2)

54(3)

26(2)

-8.0(18)

4.6(18)

-4(2)

32(2)

62(3)

49(3)

-1(2)

2(2)

-1(2)

31(2)

51(2)

43(2)

5(2)

8.2(18)

4.2(18)

C13

62(3)

42(2)

46(3)

-1(2)

7(2)

-5(2)

41(2)

39(2)

45(2)

-4.5(19)

8.6(19)

-5.9(18)

C16

51(3)

48(3)

34(2)

2.1(19)

7(2)

-4(2)

C15

55(3)

70(3)

42(3)

21(2)

3(2)

0(2)

C21

55(3)

53(3)

50(3)

9(2)

16(2)

-8(2)

49(3)

74(3)

36(2)

10(2)

1(2)

-5(2)

C26

66(3)

54(3)

45(3)

-13(2)

0(2)

C28

62(3)

57(3)

61(3)

-14(2)

27(3)

-22(2)

C14

73(3)

50(3)

59(3)

14(2)

4(3)

1(3)

69(3)

76(3)

47(3)

-4(3)

26(3)

-1(3)

C23

70(3)

84(4)

57(3)

6(3)

35(3)

-17(3)

C27

40(2)

46(3)

79(4)

-17(2)

8(2)

-14(2)

C24

55(3)

69(3)

58(3)

4(3)

27(3)

-4(2)

C11

43(3)

71(3)

78(4)

-6(3)

25(3)

14(2)

C12

77(4)

92(4)

40(3)

-22(3)

27(3)

-18(3)

C20

48(3)

59(3)

82(4)

-19(3)

24(3)

-2(2)

57(3)

41(3)

78(4)

13(2)

-1(3)

4(2)

C22

85(4)

61(3)

67(3)

11(3)

40(3)

-18(3)

59(3)

63(3)

66(3)

14(3)

27(3)

-2(2)

39(2)

70(3)

69(3)

-3(3)

21(2)

-2(2)

C19

70(4)

73(4)

-30(3)

21(3)

-3(3)

C10

71(3)

40(3)

85(4)

-23(3)

25(3)

-3(2)

C25

59(3)

68(3)

42(3)

1(2)

6(2)

-10(3)

C18

55(3)

102(5)

110(5)

-56(4)

35(3)

-15(3)

C17

40(3)

80(4)

91(4)

-26(3)

20(3)

8(3)

Li4

27(3)

34(3)

29(3)

0(3)

-4(3)

Li3

29(3)

38(3)

22(3)

-1(2)

6(2)

-3(3)

Li2

29(3)

32(3)

33(3)

-5(3)

12(3)

5(3)

Li1

28(3)

32(3)

29(3)

-3(3)

6(3)

-2(2)

Table 4 Bond Lengths for 3182.
Atom	Atom	Length/Å	Atom	Atom	Length/Å
Si3	O3	1.598(3)	O5	C16	1.429(5)
Si3	C9	1.877(4)	O5	Li1	2.024(6)
Si3	C7	1.881(5)	O7	C21	1.439(5)
Si3	C8	1.884(5)	O7	C24	1.431(5)
Si1	O1	1.597(2)	O7	Li3	2.003(7)
Si1	C2	1.888(4)	O6	C20	1.438(6)
Si1	C1	1.877(4)	O6	C17	1.444(5)
Si1	C3	1.878(4)	O6	Li2	1.973(6)
Si4	O4	1.588(3)	O8	C28	1.429(5)
Si4	C11	1.881(5)	O8	C25	1.439(5)
Si4	C12	1.881(5)	O8	Li4	1.999(6)
Si4	C10	1.880(5)	C13	C14	1.510(6)
Si2	O2	1.593(3)	C16	C15	1.515(6)
Si2	C6	1.890(5)	C15	C14	1.477(7)
Si2	C4	1.878(5)	C21	C22	1.509(7)
Si2	C5	1.880(5)	C26	C27	1.470(7)
O1	Li3	1.955(6)	C26	C25	1.516(7)
O1	Li2	1.945(6)	C28	C27	1.506(6)
O1	Li1	1.960(6)	C23	C24	1.500(7)
O4	Li4	1.936(7)	C23	C22	1.496(8)
O4	Li3	1.973(7)	C20	C19	1.492(7)
O4	Li1	1.945(6)	C19	C18	1.517(7)
O2	Li4	1.950(7)	C18	C17	1.451(7)
O2	Li2	1.971(7)	Li4	Li3	2.573(8)
O2	Li1	1.964(6)	Li4	Li2	2.584(8)
O3	Li4	1.975(7)	Li4	Li1	2.513(8)
O3	Li3	1.944(6)	Li3	Li2	2.523(8)
O3	Li2	1.956(6)	Li3	Li1	2.563(8)
O5	C13	1.436(5)	Li2	Li1	2.574(8)

Table 4 Bond Lengths for 3182.

Atom

Length/Å

Atom

Length/Å

Si3

1.598(3)

C16

1.429(5)

Si3

1.877(4)

Li1

2.024(6)

Si3

1.881(5)

C21

1.439(5)

Si3

1.884(5)

C24

1.431(5)

Si1

1.597(2)

Li3

2.003(7)

Si1

1.888(4)

C20

1.438(6)

Si1

1.877(4)

C17

1.444(5)

Si1

1.878(4)

Li2

1.973(6)

Si4

1.588(3)

C28

1.429(5)

Si4

C11

1.881(5)

C25

1.439(5)

Si4

C12

1.881(5)

Li4

1.999(6)

Si4

C10

1.880(5)

C13

C14

1.510(6)

Si2

1.593(3)

C16

C15

1.515(6)

Si2

1.890(5)

C15

C14

1.477(7)

Si2

1.878(5)

C21

C22

1.509(7)

Si2

1.880(5)

C26

C27

1.470(7)

Li3

1.955(6)

C26

C25

1.516(7)

Li2

1.945(6)

C28

C27

1.506(6)

Li1

1.960(6)

C23

C24

1.500(7)

Li4

1.936(7)

C23

C22

1.496(8)

Li3

1.973(7)

C20

C19

1.492(7)

Li1

1.945(6)

C19

C18

1.517(7)

Li4

1.950(7)

C18

C17

1.451(7)

Li2

1.971(7)

Li4

Li3

2.573(8)

Li1

1.964(6)

Li4

Li2

2.584(8)

Li4

1.975(7)

Li4

Li1

2.513(8)

Li3

1.944(6)

Li3

Li2

2.523(8)

Li2

1.956(6)

Li3

Li1

2.563(8)

C13

1.436(5)

Li2

Li1

2.574(8)

Table 5 Bond Angles for 3182.
Atom	Atom	Atom	Angle/˚	Atom	Atom	Atom	Angle/˚
O3	Si3	C9	111.96(18)	O4	Li4	Li2	95.6(3)
O3	Si3	C7	111.79(19)	O4	Li4	Li1	49.8(2)
O3	Si3	C8	112.44(18)	O2	Li4	O3	96.9(3)
C9	Si3	C7	107.4(2)	O2	Li4	O8	122.7(3)
C9	Si3	C8	106.0(2)	O2	Li4	Li3	95.5(3)
C7	Si3	C8	106.8(3)	O2	Li4	Li2	49.1(2)
O1	Si1	C2	110.99(17)	O2	Li4	Li1	50.3(2)
O1	Si1	C1	112.06(17)	O3	Li4	O8	120.5(3)
O1	Si1	C3	112.31(16)	O3	Li4	Li3	48.4(2)
C1	Si1	C2	106.83(19)	O3	Li4	Li2	48.6(2)
C1	Si1	C3	106.7(2)	O3	Li4	Li1	96.3(3)
C3	Si1	C2	107.6(2)	O8	Li4	Li3	141.8(3)
O4	Si4	C11	111.25(19)	O8	Li4	Li2	149.3(3)
O4	Si4	C12	112.0(2)	O8	Li4	Li1	142.9(3)
O4	Si4	C10	113.1(2)	Li3	Li4	Li2	58.6(2)
C12	Si4	C11	106.8(3)	Li1	Li4	Li3	60.5(2)
C10	Si4	C11	107.4(2)	Li1	Li4	Li2	60.7(2)
C10	Si4	C12	105.8(3)	O1	Li3	O4	97.2(3)
O2	Si2	C6	111.9(2)	O1	Li3	O7	115.1(3)
O2	Si2	C4	111.7(2)	O1	Li3	Li4	95.2(3)
O2	Si2	C5	112.06(19)	O1	Li3	Li2	49.5(2)
C4	Si2	C6	106.7(2)	O1	Li3	Li1	49.2(2)
C4	Si2	C5	106.1(2)	O4	Li3	O7	125.4(3)
C5	Si2	C6	108.0(2)	O4	Li3	Li4	48.2(2)
Si1	O1	Li3	130.9(2)	O4	Li3	Li2	96.5(3)
Si1	O1	Li2	137.2(2)	O4	Li3	Li1	48.7(2)
Si1	O1	Li1	124.4(2)	O3	Li3	O1	99.1(3)
Li3	O1	Li1	81.8(3)	O3	Li3	O4	96.9(3)
Li2	O1	Li3	80.6(3)	O3	Li3	O7	118.1(3)
Li2	O1	Li1	82.5(3)	O3	Li3	Li4	49.5(2)
Si4	O4	Li4	135.1(2)	O3	Li3	Li2	49.9(2)
Si4	O4	Li3	121.9(2)	O3	Li3	Li1	95.5(3)
Si4	O4	Li1	135.3(2)	O7	Li3	Li4	149.6(3)
Li4	O4	Li3	82.3(3)	O7	Li3	Li2	138.0(3)
Li4	O4	Li1	80.7(3)	O7	Li3	Li1	146.0(3)
Li1	O4	Li3	81.7(3)	Li2	Li3	Li4	60.9(2)
Si2	O2	Li4	134.8(2)	Li2	Li3	Li1	60.8(2)
Si2	O2	Li2	124.2(2)	Li1	Li3	Li4	58.6(2)
Si2	O2	Li1	134.3(2)	O1	Li2	O2	97.2(3)
Li4	O2	Li2	82.4(3)	O1	Li2	O3	99.0(3)
Li4	O2	Li1	79.9(3)	O1	Li2	O6	120.0(3)
Li1	O2	Li2	81.7(3)	O1	Li2	Li4	95.1(3)
Si3	O3	Li4	125.3(2)	O1	Li2	Li3	49.9(2)
Si3	O3	Li3	139.5(2)	O1	Li2	Li1	49.0(2)
Si3	O3	Li2	127.6(2)	O2	Li2	O6	123.4(3)
Li3	O3	Li4	82.1(3)	O2	Li2	Li4	48.4(2)
Li3	O3	Li2	80.6(3)	O2	Li2	Li3	96.5(3)
Li2	O3	Li4	82.2(3)	O2	Li2	Li1	49.0(2)
C13	O5	Li1	120.8(3)	O3	Li2	O2	96.8(3)
C16	O5	C13	109.3(3)	O3	Li2	O6	115.4(3)
C16	O5	Li1	126.8(3)	O3	Li2	Li4	49.2(2)
C21	O7	Li3	117.9(3)	O3	Li2	Li3	49.5(2)
C24	O7	C21	109.2(3)	O3	Li2	Li1	94.8(3)
C24	O7	Li3	130.9(3)	O6	Li2	Li4	144.7(3)
C20	O6	C17	106.0(3)	O6	Li2	Li3	140.0(4)
C20	O6	Li2	125.9(3)	O6	Li2	Li1	149.8(3)
C17	O6	Li2	128.1(3)	Li3	Li2	Li4	60.5(2)
C28	O8	C25	109.2(3)	Li3	Li2	Li1	60.4(2)
C28	O8	Li4	129.4(3)	Li1	Li2	Li4	58.3(2)
C25	O8	Li4	119.6(3)	O1	Li1	O2	97.0(3)
O5	C13	C14	106.1(4)	O1	Li1	O5	124.9(3)
O5	C16	C15	105.8(4)	O1	Li1	Li4	97.0(3)
C14	C15	C16	102.7(4)	O1	Li1	Li3	49.0(2)
O7	C21	C22	105.9(4)	O1	Li1	Li2	48.5(2)
C27	C26	C25	103.1(4)	O4	Li1	O1	97.9(3)
O8	C28	C27	106.0(4)	O4	Li1	O2	99.0(3)
C15	C14	C13	103.4(4)	O4	Li1	O5	116.7(3)
C22	C23	C24	102.0(4)	O4	Li1	Li4	49.5(2)
C26	C27	C28	102.5(4)	O4	Li1	Li3	49.6(2)
O7	C24	C23	105.9(4)	O4	Li1	Li2	95.6(3)
O6	C20	C19	103.3(4)	O2	Li1	O5	116.5(3)
C23	C22	C21	103.3(4)	O2	Li1	Li4	49.8(2)
C20	C19	C18	101.3(4)	O2	Li1	Li3	95.5(3)
O8	C25	C26	105.0(4)	O2	Li1	Li2	49.3(2)
C17	C18	C19	104.8(4)	O5	Li1	Li4	138.2(3)
O6	C17	C18	108.0(4)	O5	Li1	Li3	147.8(3)
O4	Li4	O2	99.8(3)	O5	Li1	Li2	147.4(3)
O4	Li4	O3	97.1(3)	Li4	Li1	Li3	60.9(2)
O4	Li4	O8	115.0(3)	Li4	Li1	Li2	61.0(2)
O4	Li4	Li3	49.5(2)	Li3	Li1	Li2	58.8(2)

Table 5 Bond Angles for 3182.

Atom

Angle/˚

Atom

Angle/˚

Si3

111.96(18)

Li4

Li2

95.6(3)

Si3

111.79(19)

Li4

Li1

49.8(2)

Si3

112.44(18)

Li4

96.9(3)

Si3

107.4(2)

Li4

122.7(3)

Si3

106.0(2)

Li4

Li3

95.5(3)

Si3

106.8(3)

Li4

Li2

49.1(2)

Si1

110.99(17)

Li4

Li1

50.3(2)

Si1

112.06(17)

Li4

120.5(3)

Si1

112.31(16)

Li4

Li3

48.4(2)

Si1

106.83(19)

Li4

Li2

48.6(2)

Si1

106.7(2)

Li4

Li1

96.3(3)

Si1

107.6(2)

Li4

Li3

141.8(3)

Si4

C11

111.25(19)

Li4

Li2

149.3(3)

Si4

C12

112.0(2)

Li4

Li1

142.9(3)

Si4

C10

113.1(2)

Li3

Li4

Li2

58.6(2)

C12

Si4

C11

106.8(3)

Li1

Li4

Li3

60.5(2)

C10

Si4

C11

107.4(2)

Li1

Li4

Li2

60.7(2)

C10

Si4

C12

105.8(3)

Li3

97.2(3)

Si2

111.9(2)

Li3

115.1(3)

Si2

111.7(2)

Li3

Li4

95.2(3)

Si2

112.06(19)

Li3

Li2

49.5(2)

Si2

106.7(2)

Li3

Li1

49.2(2)

Si2

106.1(2)

Li3

125.4(3)

Si2

108.0(2)

Li3

Li4

48.2(2)

Si1

Li3

130.9(2)

Li3

Li2

96.5(3)

Si1

Li2

137.2(2)

Li3

Li1

48.7(2)

Si1

Li1

124.4(2)

Li3

99.1(3)

Li3

Li1

81.8(3)

Li3

96.9(3)

Li2

Li3

80.6(3)

Li3

118.1(3)

Li2

Li1

82.5(3)

Li3

Li4

49.5(2)

Si4

Li4

135.1(2)

Li3

Li2

49.9(2)

Si4

Li3

121.9(2)

Li3

Li1

95.5(3)

Si4

Li1

135.3(2)

Li3

Li4

149.6(3)

Li4

Li3

82.3(3)

Li3

Li2

138.0(3)

Li4

Li1

80.7(3)

Li3

Li1

146.0(3)

Li1

Li3

81.7(3)

Li2

Li3

Li4

60.9(2)

Si2

Li4

134.8(2)

Li2

Li3

Li1

60.8(2)

Si2

Li2

124.2(2)

Li1

Li3

Li4

58.6(2)

Si2

Li1

134.3(2)

Li2

97.2(3)

Li4

Li2

82.4(3)

Li2

99.0(3)

Li4

Li1

79.9(3)

Li2

120.0(3)

Li1

Li2

81.7(3)

Li2

Li4

95.1(3)

Si3

Li4

125.3(2)

Li2

Li3

49.9(2)

Si3

Li3

139.5(2)

Li2

Li1

49.0(2)

Si3

Li2

127.6(2)

Li2

123.4(3)

Li3

Li4

82.1(3)

Li2

Li4

48.4(2)

Li3

Li2

80.6(3)

Li2

Li3

96.5(3)

Li2

Li4

82.2(3)

Li2

Li1

49.0(2)

C13

Li1

120.8(3)

Li2

96.8(3)

C16

C13

109.3(3)

Li2

115.4(3)

C16

Li1

126.8(3)

Li2

Li4

49.2(2)

C21

Li3

117.9(3)

Li2

Li3

49.5(2)

C24

C21

109.2(3)

Li2

Li1

94.8(3)

C24

Li3

130.9(3)

Li2

Li4

144.7(3)

C20

C17

106.0(3)

Li2

Li3

140.0(4)

C20

Li2

125.9(3)

Li2

Li1

149.8(3)

C17

Li2

128.1(3)

Li3

Li2

Li4

60.5(2)

C28

C25

109.2(3)

Li3

Li2

Li1

60.4(2)

C28

Li4

129.4(3)

Li1

Li2

Li4

58.3(2)

C25

Li4

119.6(3)

Li1

97.0(3)

C13

C14

106.1(4)

Li1

124.9(3)

C16

C15

105.8(4)

Li1

Li4

97.0(3)

C14

C15

C16

102.7(4)

Li1

Li3

49.0(2)

C21

C22

105.9(4)

Li1

Li2

48.5(2)

C27

C26

C25

103.1(4)

Li1

97.9(3)

C28

C27

106.0(4)

Li1

99.0(3)

C15

C14

C13

103.4(4)

Li1

116.7(3)

C22

C23

C24

102.0(4)

Li1

Li4

49.5(2)

C26

C27

C28

102.5(4)

Li1

Li3

49.6(2)

C24

C23

105.9(4)

Li1

Li2

95.6(3)

C20

C19

103.3(4)

Li1

116.5(3)

C23

C22

C21

103.3(4)

Li1

Li4

49.8(2)

C20

C19

C18

101.3(4)

Li1

Li3

95.5(3)

C25

C26

105.0(4)

Li1

Li2

49.3(2)

C17

C18

C19

104.8(4)

Li1

Li4

138.2(3)

C17

C18

108.0(4)

Li1

Li3

147.8(3)

Li4

99.8(3)

Li1

Li2

147.4(3)

Li4

97.1(3)

Li4

Li1

Li3

60.9(2)

Li4

115.0(3)

Li4

Li1

Li2

61.0(2)

Li4

Li3

49.5(2)

Li3

Li1

Li2

58.8(2)

Table 6 Torsion Angles for 3182.
A	B	C	D	Angle/˚	A	B	C	D	Angle/˚
O5	C13	C14	C15	-27.3(6)	C11	Si4	O4	Li3	74.7(3)
O5	C16	C15	C14	-31.2(5)	C11	Si4	O4	Li1	-38.1(4)
O7	C21	C22	C23	26.4(5)	C12	Si4	O4	Li4	68.8(4)
O6	C20	C19	C18	-40.3(6)	C12	Si4	O4	Li3	-44.8(3)
O8	C28	C27	C26	31.2(5)	C12	Si4	O4	Li1	-157.6(3)
C2	Si1	O1	Li3	176.2(3)	C20	O6	C17	C18	-17.3(7)
C2	Si1	O1	Li2	48.0(4)	C20	C19	C18	C17	29.7(7)
C2	Si1	O1	Li1	-72.4(3)	C8	Si3	O3	Li4	159.8(3)
C9	Si3	O3	Li4	40.5(3)	C8	Si3	O3	Li3	-75.5(4)
C9	Si3	O3	Li3	165.3(4)	C8	Si3	O3	Li2	50.2(4)
C9	Si3	O3	Li2	-69.0(3)	C22	C23	C24	O7	33.7(5)
C1	Si1	O1	Li3	-64.5(3)	C4	Si2	O2	Li4	77.6(4)
C1	Si1	O1	Li2	167.3(3)	C4	Si2	O2	Li2	-165.7(3)
C1	Si1	O1	Li1	46.9(3)	C4	Si2	O2	Li1	-50.8(4)
C13	O5	C16	C15	14.5(5)	C5	Si2	O2	Li4	-41.4(4)
C3	Si1	O1	Li3	55.7(3)	C5	Si2	O2	Li2	75.4(3)
C3	Si1	O1	Li2	-72.6(4)	C5	Si2	O2	Li1	-169.8(3)
C3	Si1	O1	Li1	167.0(3)	C19	C18	C17	O6	-8.5(7)
C16	O5	C13	C14	7.8(5)	C10	Si4	O4	Li4	-50.6(4)
C16	C15	C14	C13	35.1(6)	C10	Si4	O4	Li3	-164.3(3)
C21	O7	C24	C23	-17.9(5)	C10	Si4	O4	Li1	82.9(4)
C7	Si3	O3	Li4	-80.1(3)	C25	O8	C28	C27	-12.0(5)
C7	Si3	O3	Li3	44.7(4)	C25	C26	C27	C28	-37.2(5)
C7	Si3	O3	Li2	170.4(3)	C17	O6	C20	C19	36.4(6)
C28	O8	C25	C26	-11.4(5)	Li4	O8	C28	C27	-176.8(4)
C6	Si2	O2	Li4	-162.8(3)	Li4	O8	C25	C26	155.1(4)
C6	Si2	O2	Li2	-46.1(3)	Li3	O7	C21	C22	160.4(4)
C6	Si2	O2	Li1	68.8(4)	Li3	O7	C24	C23	178.8(4)
C27	C26	C25	O8	30.8(5)	Li2	O6	C20	C19	-141.8(4)
C24	O7	C21	C22	-5.4(5)	Li2	O6	C17	C18	160.7(5)
C24	C23	C22	C21	-36.2(5)	Li1	O5	C13	C14	-153.6(4)
C11	Si4	O4	Li4	-171.6(4)	Li1	O5	C16	C15	174.5(4)

Table 6 Torsion Angles for 3182.

Angle/˚

C13

C14

C15

-27.3(6)

C11

Si4

Li3

74.7(3)

C16

C15

C14

-31.2(5)

C11

Si4

Li1

-38.1(4)

C21

C22

C23

26.4(5)

C12

Si4

Li4

68.8(4)

C20

C19

C18

-40.3(6)

C12

Si4

Li3

-44.8(3)

C28

C27

C26

31.2(5)

C12

Si4

Li1

-157.6(3)

Si1

Li3

176.2(3)

C20

C17

C18

-17.3(7)

Si1

Li2

48.0(4)

C20

C19

C18

C17

29.7(7)

Si1

Li1

-72.4(3)

Si3

Li4

159.8(3)

Si3

Li4

40.5(3)

Si3

Li3

-75.5(4)

Si3

Li3

165.3(4)

Si3

Li2

50.2(4)

Si3

Li2

-69.0(3)

C22

C23

C24

33.7(5)

Si1

Li3

-64.5(3)

Si2

Li4

77.6(4)

Si1

Li2

167.3(3)

Si2

Li2

-165.7(3)

Si1

Li1

46.9(3)

Si2

Li1

-50.8(4)

C13

C16

C15

14.5(5)

Si2

Li4

-41.4(4)

Si1

Li3

55.7(3)

Si2

Li2

75.4(3)

Si1

Li2

-72.6(4)

Si2

Li1

-169.8(3)

Si1

Li1

167.0(3)

C19

C18

C17

-8.5(7)

C16

C13

C14

7.8(5)

C10

Si4

Li4

-50.6(4)

C16

C15

C14

C13

35.1(6)

C10

Si4

Li3

-164.3(3)

C21

C24

C23

-17.9(5)

C10

Si4

Li1

82.9(4)

Si3

Li4

-80.1(3)

C25

C28

C27

-12.0(5)

Si3

Li3

44.7(4)

C25

C26

C27

C28

-37.2(5)

Si3

Li2

170.4(3)

C17

C20

C19

36.4(6)

C28

C25

C26

-11.4(5)

Li4

C28

C27

-176.8(4)

Si2

Li4

-162.8(3)

Li4

C25

C26

155.1(4)

Si2

Li2

-46.1(3)

Li3

C21

C22

160.4(4)

Si2

Li1

68.8(4)

Li3

C24

C23

178.8(4)

C27

C26

C25

30.8(5)

Li2

C20

C19

-141.8(4)

C24

C21

C22

-5.4(5)

Li2

C17

C18

160.7(5)

C24

C23

C22

C21

-36.2(5)

Li1

C13

C14

-153.6(4)

C11

Si4

Li4

-171.6(4)

Li1

C16

C15

174.5(4)

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for 3182.
Atom	x	y	z	U(eq)
H2A	13574	11940	4432	67
H2B	14420	11758	4750	67
H2C	13907	10576	4631	67
H9A	10257	10043	1146	78
H9B	9984	11427	904	78
H9C	10346	11104	1706	78
H1A	14709	9406	3808	65
H1B	15187	10640	3968	65
H1C	14793	10172	3192	65
H13A	13821	5980	3452	65
H13B	13012	6049	3402	65
H3A	14181	12688	2821	66
H3B	14503	13181	3598	66
H3C	13666	13286	3153	66
H16A	13580	8091	4728	57
H16B	14309	8428	4635	57
H15A	14726	6440	4858	73
H15B	14261	6477	5329	73
H21A	13043	12785	1633	65
H21B	12735	12244	861	65
H7A	11653	11344	325	87
H7B	10802	11435	22	87
H7C	11186	10123	278	87
H26A	10217	6495	-15	74
H26B	10937	5830	496	74
H28A	10480	6917	1910	71
H28B	11096	6029	1861	71
H14A	13321	5523	4517	80
H14B	13969	4840	4396	80
H6A	12429	9496	4583	94
H6B	11656	9405	4614	94
H6C	11844	10544	4224	94
H23A	14672	11964	1161	80
H23B	13943	11480	566	80
H27A	10157	5240	969	71
H27B	9748	6561	800	71
H24A	14101	9974	1372	71
H24B	14459	10927	2000	71
H11A	14321	8154	2194	96
H11B	14296	6727	1968	96
H11C	14238	7078	2683	96
H12A	12402	7883	581	103
H12B	13159	7355	641	103
H12C	13086	8771	840	103
H20A	12241	14020	3164	76
H20B	12802	13097	3712	76
H8A	11453	13271	1868	100
H8B	10894	13484	1097	100
H8C	11726	13380	1253	100
H22A	13605	13426	764	81
H22B	14086	13353	1576	81
H4A	11529	6521	3341	92
H4B	11416	6854	4033	92
H4C	12200	6860	4026	92
H5A	10513	9899	3003	89
H5B	10358	8649	3335	89
H5C	10431	8603	2605	89
H19A	12108	14540	4167	87
H19B	12169	13106	4414	87
H10A	12896	5467	2172	101
H10B	12944	5287	1437	101
H10C	12233	5831	1486	101
H25A	11333	7835	619	73
H25B	10556	8392	486	73
H18A	10957	13239	3906	106
H18B	10983	14276	3364	106
H17A	10948	11760	3218	87
H17B	10848	12796	2638	87

Table 7 Hydrogen Atom Coordinates (Å×10⁴) and Isotropic Displacement Parameters (Å²×10³) for 3182.

Atom

U(eq)

H2A

13574

11940

4432

H2B

14420

11758

4750

H2C

13907

10576

4631

H9A

10257

10043

1146

H9B

9984

11427

904

H9C

10346

11104

1706

H1A

14709

9406

3808

H1B

15187

10640

3968

H1C

14793

10172

3192

H13A

13821

5980

3452

H13B

13012

6049

3402

H3A

14181

12688

2821

H3B

14503

13181

3598

H3C

13666

13286

3153

H16A

13580

8091

4728

H16B

14309

8428

4635

H15A

14726

6440

4858

H15B

14261

6477

5329

H21A

13043

12785

1633

H21B

12735

12244

861

H7A

11653

11344

325

H7B

10802

11435

H7C

11186

10123

278

H26A

10217

6495

-15

H26B

10937

5830

496

H28A

10480

6917

1910

H28B

11096

6029

1861

H14A

13321

5523

4517

H14B

13969

4840

4396

H6A

12429

9496

4583

H6B

11656

9405

4614

H6C

11844

10544

4224

H23A

14672

11964

1161

H23B

13943

11480

566

H27A

10157

5240

969

H27B

9748

6561

800

H24A

14101

9974

1372

H24B

14459

10927

2000

H11A

14321

8154

2194

H11B

14296

6727

1968

H11C

14238

7078

2683

H12A

12402

7883

581

103

H12B

13159

7355

641

103

H12C

13086

8771

840

103

H20A

12241

14020

3164

H20B

12802

13097

3712

H8A

11453

13271

1868

100

H8B

10894

13484

1097

100

H8C

11726

13380

1253

100

H22A

13605

13426

764

H22B

14086

13353

1576

H4A

11529

6521

3341

H4B

11416

6854

4033

H4C

12200

6860

4026

H5A

10513

9899

3003

H5B

10358

8649

3335

H5C

10431

8603

2605

H19A

12108

14540

4167

H19B

12169

13106

4414

H10A

12896

5467

2172

101

H10B

12944

5287

1437

101

H10C

12233

5831

1486

101

H25A

11333

7835

619

H25B

10556

8392

486

H18A

10957

13239

3906

106

H18B

10983

14276

3364

106

H17A

10948

11760

3218

H17B

10848

12796

2638

Experimental

Single crystals of C₂₈H₆₈Li₄O₈Si₄ [3182] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 K during data collection. Using Olex2 [1], the structure was solved with the SIR2004 [2] structure solution program using Direct Methods and refined with the ShelXL [3] refinement package using Least Squares minimisation.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.

Crystal structure determination of [3182]

Crystal Data for C₂₈H₆₈Li₄O₈Si₄ (M =672.94 g/mol): monoclinic, space group P2₁/c (no. 14), a = 20.3421(14) Å, b = 10.7413(5) Å, c = 21.0670(16) Å, β = 112.664(9)°, V = 4247.7(5) Å³, Z = 4, T = 173.15 K, μ(MoKα) = 0.176 mm^-1, Dcalc = 1.052 g/cm³, 46058 reflections measured (4.19° ≤ 2Θ ≤ 50°), 7469 unique (R_int = 0.0673, R_sigma = 0.0436) which were used in all calculations. The final R₁ was 0.0710 (I > 2σ(I)) and wR₂ was 0.2057 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C15(H15A,H15B), C21(H21A,H21B), C26(H26A,
 H26B), C28(H28A,H28B), C14(H14A,H14B), C23(H23A,H23B), C27(H27A,H27B),
 C24(H24A,H24B), C20(H20A,H20B), C22(H22A,H22B), C19(H19A,H19B), C25(H25A,H25B),
  C18(H18A,H18B), C17(H17A,H17B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C7(H7A,
 H7B,H7C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C8(H8A,
 H8B,H8C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C)

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