Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105026698/lc5031sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768105026698/lc5031sup2.fcf |
Data collection: SMART(Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT (Siemens, 1995)& SADABS (Sheldrick, 2001); program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL (Bruker, 2001); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXTL (Bruker, 2001).
O120Si60 | Dx = 1.754 Mg m−3 |
Mr = 3605.40 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, R3 | Cell parameters from 7657 reflections |
Hall symbol: -R 3 | θ = 2.6–28.3° |
a = 13.7761 (1) Å | µ = 0.66 mm−1 |
c = 41.5456 (6) Å | T = 183 K |
V = 6828.23 (12) Å3 | Hexagonal plate, colourless |
Z = 2 | 0.26 × 0.22 × 0.08 mm |
F(000) = 3600 |
CCD area detector diffractometer | 3622 independent reflections |
Radiation source: fine-focus sealed tube | 3556 reflections with I > 2σI |
Graphite monochromator | Rint = 0.031 |
ω scans | θmax = 28.3°, θmin = 2.6° |
Absorption correction: multi-scan SADABS (Sheldrick, 2001) | h = −18→18 |
Tmin = 0.880, Tmax = 0.949 | k = −18→18 |
44259 measured reflections | l = 0→54 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.024 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.082 | w = 1/[σ2(Fo2) + (0.0757P)2 + 2.4398P] where P = (Fo2 + 2Fc2)/3 |
S = 0.95 | (Δ/σ)max = 0.001 |
3622 reflections | Δρmax = 1.13 e Å−3 |
184 parameters | Δρmin = −0.34 e Å−3 |
O120Si60 | Z = 2 |
Mr = 3605.40 | Mo Kα radiation |
Trigonal, R3 | µ = 0.66 mm−1 |
a = 13.7761 (1) Å | T = 183 K |
c = 41.5456 (6) Å | 0.26 × 0.22 × 0.08 mm |
V = 6828.23 (12) Å3 |
CCD area detector diffractometer | 3622 independent reflections |
Absorption correction: multi-scan SADABS (Sheldrick, 2001) | 3556 reflections with I > 2σI |
Tmin = 0.880, Tmax = 0.949 | Rint = 0.031 |
44259 measured reflections |
R[F2 > 2σ(F2)] = 0.024 | 184 parameters |
wR(F2) = 0.082 | 0 restraints |
S = 0.95 | Δρmax = 1.13 e Å−3 |
3622 reflections | Δρmin = −0.34 e Å−3 |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s 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 > σ(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. |
x | y | z | Uiso*/Ueq | ||
Si1 | 0.0000 | 0.0000 | 0.13722 (2) | 0.0123 (2) | |
Si2 | 0.0000 | 0.0000 | 0.21342 (2) | 0.00817 (18) | |
Si3 | 0.13827 (5) | 0.25814 (5) | 0.232250 (13) | 0.00771 (12) | |
Si4 | 0.18478 (5) | 0.40151 (5) | 0.167658 (13) | 0.00843 (12) | |
Si5 | −0.03853 (5) | 0.29578 (5) | 0.265664 (14) | 0.00883 (12) | |
Si6 | −0.09872 (5) | 0.34502 (5) | 0.333414 (15) | 0.00889 (12) | |
Si7 | −0.01778 (5) | 0.39330 (5) | 0.402585 (13) | 0.00847 (12) | |
Si8 | −0.09487 (5) | 0.45115 (5) | 0.224061 (13) | 0.01007 (12) | |
O1 | 0.09544 (15) | 0.12081 (16) | 0.12437 (4) | 0.0209 (4) | |
O2 | 0.0000 | 0.0000 | 0.17547 (8) | 0.0495 (12) | |
O3 | 0.07050 (17) | 0.12578 (15) | 0.22611 (5) | 0.0282 (4) | |
O4 | 0.15270 (17) | 0.32494 (16) | 0.19927 (3) | 0.0206 (4) | |
O5 | 0.07297 (15) | 0.29034 (15) | 0.25830 (4) | 0.0162 (3) | |
O6 | −0.03693 (15) | 0.33004 (16) | 0.30274 (4) | 0.0182 (3) | |
O7 | −0.02068 (14) | 0.36753 (15) | 0.36467 (4) | 0.0167 (4) | |
O8 | −0.03934 (17) | 0.38815 (16) | 0.24238 (5) | 0.0220 (4) | |
O9 | 0.12607 (15) | 0.32187 (16) | 0.13710 (4) | 0.0176 (3) | |
O10 | 0.31761 (14) | 0.47062 (15) | 0.16245 (4) | 0.0201 (4) | |
O11 | 0.25985 (14) | 0.29461 (14) | 0.24666 (4) | 0.0143 (3) | |
O12 | −0.14638 (15) | 0.17497 (15) | 0.25858 (4) | 0.0208 (4) | |
O13 | −0.11907 (17) | 0.44852 (16) | 0.32776 (4) | 0.0241 (4) | |
O14 | −0.11701 (14) | 0.52702 (14) | 0.24908 (4) | 0.0169 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Si1 | 0.0136 (3) | 0.0136 (3) | 0.0098 (4) | 0.00681 (15) | 0.000 | 0.000 |
Si2 | 0.0074 (3) | 0.0074 (3) | 0.0098 (4) | 0.00368 (13) | 0.000 | 0.000 |
Si3 | 0.0068 (2) | 0.0074 (3) | 0.0089 (2) | 0.0036 (2) | −0.0001 (2) | 0.00036 (19) |
Si4 | 0.0085 (3) | 0.0106 (3) | 0.0079 (2) | 0.0060 (2) | −0.0008 (2) | 0.0000 (2) |
Si5 | 0.0082 (3) | 0.0098 (3) | 0.0086 (2) | 0.0045 (2) | 0.0012 (2) | 0.0007 (2) |
Si6 | 0.0097 (3) | 0.0084 (3) | 0.0079 (2) | 0.0040 (2) | 0.0002 (2) | −0.00097 (19) |
Si7 | 0.0088 (3) | 0.0097 (3) | 0.0078 (2) | 0.0053 (2) | −0.0007 (2) | 0.0006 (2) |
Si8 | 0.0111 (3) | 0.0087 (3) | 0.0104 (2) | 0.0049 (2) | 0.0009 (2) | 0.0006 (2) |
O1 | 0.0148 (8) | 0.0133 (8) | 0.0331 (9) | 0.0059 (7) | −0.0055 (7) | 0.0050 (7) |
O2 | 0.0698 (19) | 0.0698 (19) | 0.0088 (13) | 0.0349 (10) | 0.000 | 0.000 |
O3 | 0.0231 (10) | 0.0099 (8) | 0.0480 (11) | 0.0055 (8) | −0.0048 (9) | −0.0067 (8) |
O4 | 0.0223 (9) | 0.0296 (10) | 0.0109 (7) | 0.0137 (8) | 0.0011 (7) | 0.0091 (7) |
O5 | 0.0127 (8) | 0.0265 (9) | 0.0129 (8) | 0.0125 (7) | 0.0022 (6) | −0.0009 (7) |
O6 | 0.0167 (8) | 0.0262 (9) | 0.0128 (7) | 0.0115 (7) | 0.0008 (6) | −0.0049 (7) |
O7 | 0.0158 (8) | 0.0276 (9) | 0.0076 (7) | 0.0115 (7) | −0.0024 (6) | −0.0023 (6) |
O8 | 0.0241 (9) | 0.0222 (9) | 0.0235 (9) | 0.0145 (8) | 0.0014 (7) | 0.0091 (7) |
O9 | 0.0185 (8) | 0.0220 (9) | 0.0135 (7) | 0.0109 (7) | −0.0028 (6) | −0.0069 (7) |
O10 | 0.0082 (8) | 0.0250 (9) | 0.0243 (9) | 0.0063 (7) | 0.0004 (6) | 0.0059 (7) |
O11 | 0.0102 (7) | 0.0192 (8) | 0.0155 (7) | 0.0087 (6) | −0.0026 (6) | 0.0012 (6) |
O12 | 0.0133 (8) | 0.0149 (8) | 0.0250 (8) | 0.0002 (7) | 0.0025 (7) | −0.0042 (7) |
O13 | 0.0374 (11) | 0.0183 (9) | 0.0244 (8) | 0.0198 (9) | −0.0032 (8) | −0.0019 (7) |
O14 | 0.0185 (8) | 0.0107 (8) | 0.0161 (8) | 0.0032 (7) | 0.0072 (7) | −0.0018 (6) |
Si1—O2i | 1.589 (3) | Si5—O12 | 1.6098 (18) |
Si1—O2 | 1.589 (3) | Si6—O13 | 1.6020 (19) |
Si1—O1ii | 1.6111 (19) | Si6—O6 | 1.6020 (18) |
Si1—O1 | 1.6111 (19) | Si6—O13iv | 1.6052 (19) |
Si1—O1i | 1.6111 (19) | Si6—O7 | 1.6138 (17) |
Si2—O2i | 1.577 (3) | Si7—O11v | 1.5995 (16) |
Si2—O2 | 1.577 (3) | Si7—O12vi | 1.6011 (18) |
Si2—O3 | 1.5939 (18) | Si7—O14iv | 1.6098 (17) |
Si2—O3ii | 1.5939 (18) | Si7—O7 | 1.6108 (16) |
Si2—O3i | 1.5939 (18) | Si8—O9iii | 1.6051 (17) |
Si3—O3 | 1.5998 (19) | Si8—O1iii | 1.606 (2) |
Si3—O11 | 1.6046 (17) | Si8—O8 | 1.6069 (18) |
Si3—O5 | 1.6051 (16) | Si8—O14 | 1.6076 (17) |
Si3—O4 | 1.6063 (16) | O1—Si8vii | 1.6057 (19) |
Si4—O10 | 1.5998 (17) | O2—O2i | 0.000 (6) |
Si4—O4 | 1.6022 (16) | O9—Si8vii | 1.6050 (17) |
Si4—O10iii | 1.6053 (16) | O10—Si4vii | 1.6052 (16) |
Si4—O9 | 1.6070 (17) | O11—Si7v | 1.5996 (16) |
Si5—O8 | 1.6029 (18) | O12—Si7iv | 1.6011 (18) |
Si5—O5 | 1.6042 (17) | O13—Si6vi | 1.6052 (19) |
Si5—O6 | 1.6081 (18) | O14—Si7vi | 1.6098 (17) |
O2i—Si1—O1ii | 109.36 (7) | O5—Si5—O12 | 109.10 (10) |
O2—Si1—O1ii | 109.36 (7) | O6—Si5—O12 | 110.41 (9) |
O2i—Si1—O1 | 109.36 (7) | O13—Si6—O6 | 109.80 (10) |
O2—Si1—O1 | 109.36 (7) | O13—Si6—O13iv | 108.34 (15) |
O1ii—Si1—O1 | 109.58 (7) | O6—Si6—O13iv | 110.40 (10) |
O2i—Si1—O1i | 109.36 (7) | O13—Si6—O7 | 110.07 (10) |
O2—Si1—O1i | 109.36 (7) | O6—Si6—O7 | 108.60 (9) |
O1ii—Si1—O1i | 109.58 (7) | O13iv—Si6—O7 | 109.63 (10) |
O1—Si1—O1i | 109.58 (7) | O11v—Si7—O12vi | 109.87 (10) |
O2i—Si2—O3 | 109.31 (8) | O11v—Si7—O14iv | 109.44 (9) |
O2—Si2—O3 | 109.31 (8) | O12vi—Si7—O14iv | 108.90 (10) |
O2i—Si2—O3ii | 109.31 (8) | O11v—Si7—O7 | 109.71 (9) |
O2—Si2—O3ii | 109.31 (8) | O12vi—Si7—O7 | 110.18 (10) |
O3—Si2—O3ii | 109.63 (8) | O14iv—Si7—O7 | 108.71 (10) |
O2i—Si2—O3i | 109.31 (8) | O9iii—Si8—O1iii | 110.52 (10) |
O2—Si2—O3i | 109.31 (8) | O9iii—Si8—O8 | 109.13 (10) |
O3—Si2—O3i | 109.63 (8) | O1iii—Si8—O8 | 108.72 (11) |
O3ii—Si2—O3i | 109.63 (8) | O9iii—Si8—O14 | 109.60 (9) |
O3—Si3—O11 | 109.83 (10) | O1iii—Si8—O14 | 108.89 (10) |
O3—Si3—O5 | 109.52 (11) | O8—Si8—O14 | 109.95 (10) |
O11—Si3—O5 | 107.66 (9) | Si8vii—O1—Si1 | 145.60 (12) |
O3—Si3—O4 | 110.58 (10) | Si2—O2—Si1 | 180.0 |
O11—Si3—O4 | 109.15 (10) | Si2—O3—Si3 | 169.40 (15) |
O5—Si3—O4 | 110.04 (10) | Si4—O4—Si3 | 172.19 (14) |
O10—Si4—O4 | 111.08 (10) | Si5—O5—Si3 | 145.43 (12) |
O10—Si4—O10iii | 109.83 (14) | Si6—O6—Si5 | 150.41 (13) |
O4—Si4—O10iii | 109.40 (11) | Si7—O7—Si6 | 140.35 (12) |
O10—Si4—O9 | 109.57 (10) | Si5—O8—Si8 | 155.35 (14) |
O4—Si4—O9 | 108.62 (10) | Si8vii—O9—Si4 | 152.27 (12) |
O10iii—Si4—O9 | 108.29 (9) | Si4—O10—Si4vii | 163.57 (12) |
O8—Si5—O5 | 107.99 (10) | Si7v—O11—Si3 | 154.76 (12) |
O8—Si5—O6 | 110.46 (11) | Si7iv—O12—Si5 | 153.67 (12) |
O5—Si5—O6 | 108.87 (9) | Si6—O13—Si6vi | 159.21 (13) |
O8—Si5—O12 | 109.95 (10) | Si8—O14—Si7vi | 148.69 (11) |
O2i—Si1—O1—Si8vii | −102.7 (2) | O6—Si6—O7—Si7 | 177.87 (17) |
O2—Si1—O1—Si8vii | −102.7 (2) | O13iv—Si6—O7—Si7 | −61.4 (2) |
O1ii—Si1—O1—Si8vii | 17.2 (3) | O5—Si5—O8—Si8 | 163.2 (3) |
O1i—Si1—O1—Si8vii | 137.45 (14) | O6—Si5—O8—Si8 | −77.9 (3) |
O2i—Si2—O3—Si3 | 17.4 (8) | O12—Si5—O8—Si8 | 44.2 (4) |
O2—Si2—O3—Si3 | 17.4 (8) | O9iii—Si8—O8—Si5 | −165.3 (3) |
O3ii—Si2—O3—Si3 | −102.4 (9) | O1iii—Si8—O8—Si5 | −44.7 (4) |
O3i—Si2—O3—Si3 | 137.2 (8) | O14—Si8—O8—Si5 | 74.4 (4) |
O11—Si3—O3—Si2 | −126.7 (8) | O10—Si4—O9—Si8vii | 39.6 (3) |
O5—Si3—O3—Si2 | 115.2 (8) | O4—Si4—O9—Si8vii | −81.9 (3) |
O4—Si3—O3—Si2 | −6.2 (8) | O10iii—Si4—O9—Si8vii | 159.4 (3) |
O8—Si5—O5—Si3 | −66.6 (2) | O4—Si4—O10—Si4vii | 6.9 (5) |
O6—Si5—O5—Si3 | 173.5 (2) | O10iii—Si4—O10—Si4vii | 128.1 (5) |
O12—Si5—O5—Si3 | 52.9 (2) | O9—Si4—O10—Si4vii | −113.1 (5) |
O3—Si3—O5—Si5 | −65.9 (2) | O3—Si3—O11—Si7v | −19.1 (3) |
O11—Si3—O5—Si5 | 174.7 (2) | O5—Si3—O11—Si7v | 100.1 (3) |
O4—Si3—O5—Si5 | 55.9 (2) | O4—Si3—O11—Si7v | −140.5 (3) |
O13—Si6—O6—Si5 | −70.3 (3) | O8—Si5—O12—Si7iv | −90.9 (3) |
O13iv—Si6—O6—Si5 | 49.1 (3) | O5—Si5—O12—Si7iv | 150.9 (3) |
O7—Si6—O6—Si5 | 169.3 (2) | O6—Si5—O12—Si7iv | 31.3 (3) |
O8—Si5—O6—Si6 | 72.2 (3) | O6—Si6—O13—Si6vi | −117.9 (4) |
O5—Si5—O6—Si6 | −169.4 (3) | O13iv—Si6—O13—Si6vi | 121.4 (4) |
O12—Si5—O6—Si6 | −49.6 (3) | O7—Si6—O13—Si6vi | 1.6 (4) |
O11v—Si7—O7—Si6 | 164.26 (18) | O9iii—Si8—O14—Si7vi | −19.9 (3) |
O12vi—Si7—O7—Si6 | −74.6 (2) | O1iii—Si8—O14—Si7vi | −140.9 (2) |
O14iv—Si7—O7—Si6 | 44.6 (2) | O8—Si8—O14—Si7vi | 100.1 (2) |
O13—Si6—O7—Si7 | 57.6 (2) |
Symmetry codes: (i) −x+y, −x, z; (ii) −y, x−y, z; (iii) y−1/3, −x+y+1/3, −z+1/3; (iv) y−2/3, −x+y−1/3, −z+2/3; (v) −x+1/3, −y+2/3, −z+2/3; (vi) x−y+1/3, x+2/3, −z+2/3; (vii) x−y+2/3, x+1/3, −z+1/3. |
Experimental details
Crystal data | |
Chemical formula | O120Si60 |
Mr | 3605.40 |
Crystal system, space group | Trigonal, R3 |
Temperature (K) | 183 |
a, c (Å) | 13.7761 (1), 41.5456 (6) |
V (Å3) | 6828.23 (12) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.66 |
Crystal size (mm) | 0.26 × 0.22 × 0.08 |
Data collection | |
Diffractometer | CCD area detector diffractometer |
Absorption correction | Multi-scan SADABS (Sheldrick, 2001) |
Tmin, Tmax | 0.880, 0.949 |
No. of measured, independent and observed (I > 2σI) reflections | 44259, 3622, 3556 |
Rint | 0.031 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.082, 0.95 |
No. of reflections | 3622 |
No. of parameters | 184 |
Δρmax, Δρmin (e Å−3) | 1.13, −0.34 |
Computer programs: SMART(Siemens, 1995), SAINT (Siemens, 1995)& SADABS (Sheldrick, 2001), SHELXTL (Bruker, 2001), DIAMOND (Brandenburg, 2005).