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The crystal structures of tert-butyl-tris(trimethylsilyl)silane, Si[C(CH_3)_3]_1[Si(CH_3)_3]_3 (Bu1), and di-tert-butyl-bis(trimethylsilyl)silane, Si[C(CH_3)_3]_2[Si(CH_3)_3]_2 (Bu2), at room temperature and at 105 K have been determined by X-ray powder diffraction; the high-pressure behavior for pressures between 0 and 5 GPa is reported. The room-temperature structures have cubic Fm\bar{3}m symmetry (Z = 4) with a = 13.2645 (2) Å, V = 2333.87 (4) Å3 for Bu1 and a = 12.9673 (1) Å, V = 2180.46 (3) Å3 for Bu2. The molecules are arranged in a cubic close packing (c.c.p.) and exhibit at least 48-fold orientational disorder. Upon cooling both compounds undergo a first-order phase transition at temperatures T_c = 230 (5) K (Bu1) and T_c = 250 (5) K (Bu2) into monoclinic structures with space group P2_1/n. The structures at 105 K have a = 17.317 (1), b = 15.598 (1), c = 16.385 (1) Å, \gamma = 109.477 (4)°, V = 4172.7 (8) Å3 and Z = 8 for Bu1and a = 17.0089 (9), b = 15.3159 (8), c = 15.9325 (8) Å, \gamma = 110.343 (3)°, V = 3891.7 (5) Å3 and Z = 8 for Bu2. The severe disorder of the room-temperature phase is significantly decreased and only a two- or threefold rotational disorder of the molecules remains at 105 K. First-order phase transitions have been observed at pressures of 0.13-0.28 GPa for Bu1 and 0.20-0.24 GPa for Bu2. The high-pressure structures are isostructural to the low-temperature structures. The pressure dependencies of the unit-cell volumes were fitted with Vinet equations of state and the bulk moduli were obtained. At still higher pressures further anomalies in the pressure dependencies of the lattice parameters were observed. These anomalies are explained as additional disorder-order phase transitions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768102021791/os0101sup1.cif
Contains datablocks global, 1, 2at105, 2at295

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768102021791/os01011sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768102021791/os01012at105sup3.hkl
Contains datablock 2at105

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768102021791/os01012at295sup4.hkl
Contains datablock 2at295

CCDC references: 205164; 205165

Computing details top

For all compounds, data collection: SPEC package ESRF; cell refinement: JANA2000. Program(s) used to solve structure: DASH for (1), 2at105. For all compounds, program(s) used to refine structure: JANA2000; software used to prepare material for publication: JANA2000.

(1) top
Crystal data top
C13H36Si4Z = 8
Mr = 304.8F(000) = 1245
Monoclinic, P_1_1_21/nDx = 0.970 (1) Mg m3
a = 17.317 (1) ÅSynchrotron radiation, λ = 0.399828(2) Å
b = 15.598 (1) ŵ = 0.22 mm1
c = 16.385 (1) ÅT = 105 K
β = 90°colourless
V = 4172.7 (5) Å3cylinder, 0.5 × 0.5 mm
Data collection top
Two-circle
diffractometer
Data collection mode: transmission
Radiation source: synchrotron, ESRF beamline BM16Scan method: continuous
Si(111) monochromator2θmin = 1.4°, 2θmax = 13.997°, 2θstep = 0.003°
Specimen mounting: lithiumborate glass capillary 0.5 mm diameter
Refinement top
Refinement on Inet60 parameters
Rp = 0.0666 restraints
Rwp = 0.08473 constraints
Rexp = 0.145H-atom parameters not defined
R(F) = 0.068Weighting scheme based on measured s.u.'s
4200 data pointsBackground function: Manual background combined with 5 terms Legendre polynomial
Profile function: Pseudo-VoigtPreferred orientation correction: none
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Si0a0.1553 (7)0.2422 (9)0.3867 (8)0.073 (7)*
C11a0.1151 (8)0.2906 (10)0.4739 (9)0.037 (4)*0.507
C111a0.1881 (11)0.3779 (12)0.5095 (10)0.041 (6)*0.659
C111/1a0.0395 (9)0.3220 (10)0.4423 (11)0.041 (6)*0.659
C111/2a0.0833 (11)0.2134 (12)0.5444 (11)0.041 (6)*0.659
C11d0.1776 (8)0.1412 (11)0.4259 (8)0.037 (4)*0.493
C111d0.1259 (9)0.0525 (13)0.3729 (10)0.041 (6)*0.641
C111/1d0.2752 (11)0.1588 (12)0.4169 (9)0.041 (6)*0.641
C111/2d0.1509 (11)0.1262 (13)0.5214 (10)0.041 (6)*0.641
Si0e0.3431 (9)0.7714 (12)0.6135 (9)0.073 (7)*
C11e0.2856 (10)0.8454 (12)0.5771 (9)0.037 (4)*0.506
C111e0.2128 (11)0.8399 (13)0.6418 (11)0.041 (6)*0.6574
C111/1e0.3480 (12)0.9494 (14)0.5705 (9)0.041 (6)*0.6574
C111/2e0.2466 (12)0.8100 (15)0.4880 (11)0.041 (6)*0.6574
C11f0.2720 (10)0.6622 (13)0.6534 (9)0.037 (4)*0.278
C111f0.1929 (12)0.6800 (14)0.6938 (9)0.041 (6)*0.3614
C111/1f0.2430 (10)0.5902 (14)0.5784 (12)0.041 (6)*0.3614
C111/2f0.3193 (11)0.6229 (14)0.7220 (12)0.041 (6)*0.3614
C11g0.4012 (10)0.7291 (12)0.5373 (9)0.037 (4)*0.216
C111g0.4232 (10)0.6443 (14)0.5765 (11)0.041 (6)*0.2812
C111/1g0.3450 (12)0.6959 (12)0.4562 (11)0.041 (6)*0.2812
C111/2g0.4850 (12)0.8110 (13)0.5141 (12)0.041 (6)*0.2812
Si21a0.1042 (8)0.3038 (9)0.4975 (9)0.037 (4)*0.493
C211a0.1774 (8)0.3186 (9)0.5895 (9)0.041 (6)*0.641
C211/1a0.0973 (8)0.4205 (10)0.4664 (9)0.041 (6)*0.641
C211/2a0.0034 (8)0.2221 (10)0.5264 (9)0.041 (6)*0.641
Si21b0.0586 (8)0.2008 (9)0.2797 (8)0.037 (4)*
C211b0.0577 (8)0.3091 (11)0.2230 (9)0.041 (6)*
C211/1b0.0885 (8)0.1213 (10)0.2049 (9)0.041 (6)*
C211/2b0.0487 (8)0.1384 (10)0.3247 (9)0.041 (6)*
Si21c0.2749 (8)0.3427 (10)0.3261 (8)0.037 (4)*
C211c0.2538 (8)0.4507 (10)0.2897 (8)0.041 (6)*
C211/1c0.3624 (8)0.3754 (10)0.4056 (9)0.041 (6)*
C211/2c0.3054 (9)0.2834 (10)0.2340 (9)0.041 (6)*
Si21d0.1837 (7)0.1139 (10)0.4365 (8)0.037 (4)*0.507
C211d0.0825 (9)0.0224 (10)0.4697 (8)0.041 (6)*0.659
C211/1d0.2349 (8)0.0661 (10)0.3513 (9)0.041 (6)*0.659
C211/2d0.2567 (8)0.1495 (10)0.5290 (9)0.041 (6)*0.659
Si21e0.2700 (9)0.8654 (12)0.5673 (9)0.037 (4)*0.494
C211e0.2585 (9)0.9420 (12)0.6560 (10)0.041 (6)*0.6426
C211/1e0.3293 (10)0.9402 (12)0.4784 (9)0.041 (6)*0.6426
C211/2e0.1629 (10)0.7903 (12)0.5300 (10)0.041 (6)*0.6426
Si21f0.2527 (9)0.6326 (12)0.6642 (9)0.037 (4)*0.722
C211f0.2169 (9)0.6517 (12)0.7723 (10)0.041 (6)*0.9386
C211/1f0.1591 (10)0.5892 (12)0.5924 (9)0.041 (6)*0.9386
C211/2f0.3089 (10)0.5444 (12)0.6688 (10)0.041 (6)*0.9386
Si21g0.4169 (9)0.7177 (12)0.5167 (9)0.037 (4)*0.784
C211g0.4610 (9)0.6328 (12)0.5689 (10)0.041 (6)*
C211/1g0.3442 (10)0.6574 (12)0.4292 (9)0.041 (6)*
C211/2g0.5054 (10)0.8192 (12)0.4736 (10)0.041 (6)*
Si21h0.4368 (9)0.8365 (12)0.7193 (9)0.037 (4)*
C211h0.3770 (10)0.8406 (12)0.8180 (10)0.041 (6)*
C211/1h0.5060 (10)0.7633 (12)0.7371 (9)0.041 (6)*
C211/2h0.5034 (10)0.9584 (12)0.6884 (9)0.041 (6)*
Geometric parameters (Å, º) top
Si0a—C11a1.86 (2)C11g—C111/1g1.63 (2)
Si0a—C11d1.86 (2)C11g—C111/2g1.63 (2)
Si0a—Si21a2.36 (2)Si21a—C211a1.93 (2)
Si0a—Si21b2.359 (18)Si21a—C211/1a1.93 (2)
Si0a—Si21c2.359 (17)Si21a—C211/2a1.933 (17)
Si0a—Si21d2.36 (2)Si21b—C211b1.93 (2)
C11a—C111a1.63 (2)Si21b—C211/1b1.93 (2)
C11a—C111/1a1.63 (2)Si21b—C211/2b1.933 (18)
C11a—C111/2a1.63 (2)Si21c—C211c1.93 (2)
C11d—C111d1.63 (2)Si21c—C211/1c1.93 (2)
C11d—C111/1d1.63 (2)Si21c—C211/2c1.93 (2)
C11d—C111/2d1.63 (2)Si21d—C211d1.933 (17)
Si0e—C11e1.86 (3)Si21d—C211/1d1.93 (2)
Si0e—C11f1.86 (2)Si21d—C211/2d1.933 (19)
Si0e—C11g1.86 (2)Si21e—C211e1.93 (2)
Si0e—Si21e2.36 (3)Si21e—C211/1e1.93 (2)
Si0e—Si21f2.36 (2)Si21e—C211/2e1.93 (2)
Si0e—Si21g2.36 (2)Si21f—C211f1.93 (2)
Si0e—Si21h2.36 (2)Si21f—C211/1f1.93 (2)
C11e—C111e1.63 (3)Si21f—C211/2f1.93 (3)
C11e—C111/1e1.63 (2)Si21g—C211g1.93 (3)
C11e—C111/2e1.63 (2)Si21g—C211/1g1.93 (2)
C11f—C111f1.63 (3)Si21g—C211/2g1.93 (2)
C11f—C111/1f1.63 (3)Si21h—C211h1.93 (2)
C11f—C111/2f1.63 (3)Si21h—C211/1h1.93 (3)
C11g—C111g1.63 (3)Si21h—C211/2h1.93 (2)
C11a—Si0a—C11d106.9 (9)Si21e—Si0e—Si21h113.8 (9)
C11a—Si0a—Si21a0Si21f—Si0e—Si21g100.5 (9)
C11a—Si0a—Si21b110.8 (9)Si21f—Si0e—Si21h106.7 (8)
C11a—Si0a—Si21c114.7 (8)Si21g—Si0e—Si21h105.7 (8)
C11a—Si0a—Si21d106.9 (8)C111e—C11e—C111/1e110.0 (14)
C11d—Si0a—Si21a106.9 (8)C111e—C11e—C111/2e110.0 (13)
C11d—Si0a—Si21b110.8 (8)C111/1e—C11e—C111/2e110.0 (12)
C11d—Si0a—Si21c108.9 (8)C111f—C11f—C111/1f110.0 (12)
C11d—Si0a—Si21d0C111f—C11f—C111/2f110.0 (13)
Si21a—Si0a—Si21b110.8 (8)C111/1f—C11f—C111/2f110.0 (16)
Si21a—Si0a—Si21c114.7 (7)C111g—C11g—C111/1g110.0 (14)
Si21a—Si0a—Si21d106.9 (7)C111g—C11g—C111/2g110.0 (14)
Si21b—Si0a—Si21c104.8 (7)C111/1g—C11g—C111/2g110.0 (13)
Si21b—Si0a—Si21d110.8 (7)C211a—Si21a—C211/1a109.7 (9)
Si21c—Si0a—Si21d108.9 (8)C211a—Si21a—C211/2a109.7 (9)
C111a—C11a—C111/1a110.0 (13)C211/1a—Si21a—C211/2a109.7 (10)
C111a—C11a—C111/2a110.0 (12)C211b—Si21b—C211/1b109.7 (9)
C111/1a—C11a—C111/2a110.0 (12)C211b—Si21b—C211/2b109.7 (10)
C111d—C11d—C111/1d110.0 (13)C211/1b—Si21b—C211/2b109.7 (9)
C111d—C11d—C111/2d110.0 (11)C211c—Si21c—C211/1c109.7 (9)
C111/1d—C11d—C111/2d110.0 (12)C211c—Si21c—C211/2c109.7 (9)
C11e—Si0e—C11f110.7 (11)C211/1c—Si21c—C211/2c109.7 (10)
C11e—Si0e—C11g118.1 (10)C211d—Si21d—C211/1d109.7 (9)
C11e—Si0e—Si21e0C211d—Si21d—C211/2d109.7 (9)
C11e—Si0e—Si21f110.7 (9)C211/1d—Si21d—C211/2d109.7 (9)
C11e—Si0e—Si21g118.1 (9)C211e—Si21e—C211/1e109.7 (11)
C11e—Si0e—Si21h113.8 (10)C211e—Si21e—C211/2e109.7 (11)
C11f—Si0e—C11g100.5 (11)C211/1e—Si21e—C211/2e109.7 (10)
C11f—Si0e—Si21e110.7 (10)C211f—Si21f—C211/1f109.7 (10)
C11f—Si0e—Si21f0C211f—Si21f—C211/2f109.7 (11)
C11f—Si0e—Si21g100.5 (10)C211/1f—Si21f—C211/2f109.7 (11)
C11f—Si0e—Si21h106.7 (9)C211g—Si21g—C211/1g109.7 (11)
C11g—Si0e—Si21e118.1 (10)C211g—Si21g—C211/2g109.7 (11)
C11g—Si0e—Si21f100.5 (10)C211/1g—Si21g—C211/2g109.7 (10)
C11g—Si0e—Si21g0C211h—Si21h—C211/1h109.7 (11)
C11g—Si0e—Si21h105.7 (10)C211h—Si21h—C211/2h109.7 (11)
Si21e—Si0e—Si21f110.7 (8)C211/1h—Si21h—C211/2h109.7 (10)
Si21e—Si0e—Si21g118.1 (8)
(2at105) top
Crystal data top
C14H36Si3Z = 8
Mr = 288.7F(000) = 1181
Monoclinic, P_1_1_21/nDx = 0.986 (1) Mg m3
a = 17.0089 (9) ÅSynchrotron radiation, λ = 0.399828(2) Å
b = 15.3159 (8) ŵ = 0.18 mm1
c = 15.9325 (8) ÅT = 105 K
β = 90°colourless
V = 3891.7 (5) Å3cylinder, 0.5 × 0.5 mm
Data collection top
Two-circle
diffractometer
Data collection mode: transmission
Radiation source: synchrotron, ESRF beamline BM16Scan method: continuous
Si(111) monochromator2θmin = 0.5°, 2θmax = 13.997°, 2θstep = 0.003°
Specimen mounting: lithiumborate glass capillary 0.5 mm diameter
Refinement top
Refinement on Inet6 restraints
Rp = 0.06759 constraints
Rwp = 0.089H-atom parameters not defined
R(F) = 0.078Weighting scheme based on measured s.u.'s
4500 data pointsBackground function: Manual background combined with 5 terms Legendre polynomial
Profile function: Pseudo-VoigtPreferred orientation correction: none
74 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Si0a0.1469 (8)0.2438 (8)0.3627 (7)0.061 (5)*
C11a0.1218 (8)0.3217 (8)0.4500 (8)0.064 (5)*0.534
C111a0.1408 (8)0.4326 (10)0.4139 (9)0.019 (4)*0.6945
C111/1a0.0187 (9)0.2763 (9)0.4800 (8)0.019 (4)*0.6945
C111/2a0.1826 (9)0.3286 (10)0.5373 (8)0.019 (4)*0.6945
C11b0.0758 (8)0.1970 (8)0.2631 (8)0.064 (5)*
C111b0.0751 (8)0.2872 (10)0.1997 (8)0.019 (4)*
C111/1b0.1119 (9)0.1244 (8)0.2052 (8)0.019 (4)*
C111/2b0.0256 (9)0.1360 (9)0.2918 (8)0.019 (4)*
C11c0.2382 (8)0.3649 (9)0.3496 (7)0.064 (5)*0.284
C111c0.3073 (9)0.3854 (9)0.4318 (9)0.019 (4)*0.3687
C111/1c0.2928 (9)0.3679 (9)0.2586 (8)0.019 (4)*0.3687
C111/2c0.1991 (9)0.4541 (9)0.3463 (9)0.019 (4)*0.3687
C11d0.1451 (8)0.1578 (9)0.4556 (8)0.064 (5)*0.182
C111d0.2351 (9)0.1315 (9)0.4566 (8)0.019 (4)*0.2367
C111/1d0.1367 (8)0.2065 (9)0.5506 (9)0.019 (4)*0.2367
C111/2d0.0617 (9)0.0557 (9)0.4458 (9)0.019 (4)*0.2367
Si0e0.3413 (7)0.7739 (7)0.6184 (7)0.061 (5)*
C11e0.3000 (7)0.8669 (8)0.5666 (7)0.064 (5)*0.796
C111e0.3646 (8)0.9241 (8)0.4863 (8)0.019 (4)*
C111/1e0.2013 (8)0.8146 (9)0.5264 (7)0.019 (4)*
C111/2e0.2960 (9)0.9481 (9)0.6388 (8)0.019 (4)*
C11f0.2631 (8)0.6743 (8)0.6874 (7)0.064 (5)*0.770
C111f0.3163 (9)0.6189 (8)0.7459 (7)0.019 (4)*
C111/1f0.2081 (8)0.7187 (9)0.7550 (8)0.019 (4)*
C111/2f0.1924 (8)0.5927 (9)0.6254 (8)0.019 (4)*
C11g0.3946 (7)0.7416 (7)0.5189 (7)0.064 (5)*0.434
C111g0.4879 (8)0.8280 (9)0.4965 (8)0.019 (4)*0.5648
C111/1g0.4143 (7)0.6405 (8)0.5353 (8)0.019 (4)*0.5648
C111/2g0.3310 (8)0.7261 (9)0.4326 (8)0.019 (4)*0.5648
Si21a0.0964 (8)0.3025 (8)0.4812 (8)0.064 (5)*0.466
C211a0.0539 (8)0.4008 (9)0.4456 (9)0.019 (4)*0.6055
C211/1a0.0052 (9)0.2015 (10)0.5349 (8)0.019 (4)*0.6055
C211/2a0.1877 (9)0.3546 (10)0.5625 (9)0.019 (4)*0.6055
Si21c0.2818 (8)0.3597 (9)0.3472 (7)0.064 (5)*0.716
C211c0.3516 (9)0.3579 (9)0.4451 (9)0.019 (4)*0.9313
C211/1c0.3358 (9)0.3353 (10)0.2452 (8)0.019 (4)*0.9313
C211/2c0.2712 (9)0.4831 (10)0.3383 (9)0.019 (4)*0.9313
Si21d0.1793 (8)0.1107 (9)0.4029 (7)0.064 (5)*0.818
C211d0.2783 (9)0.1081 (9)0.3408 (8)0.019 (4)*
C211/1d0.2029 (8)0.1154 (10)0.5239 (9)0.019 (4)*
C211/2d0.0838 (9)0.0029 (10)0.3777 (9)0.019 (4)*
Si21e0.2572 (7)0.8682 (8)0.6009 (7)0.064 (5)*0.204
C211e0.3283 (9)1.0004 (10)0.6040 (7)0.019 (4)*0.2655
C211/1e0.1987 (8)0.8405 (8)0.4925 (8)0.019 (4)*0.2655
C211/2e0.1739 (9)0.8428 (9)0.6917 (8)0.019 (4)*0.2655
Si21f0.2241 (8)0.6414 (8)0.6562 (7)0.064 (5)*0.230
C211f0.2104 (8)0.6363 (9)0.7789 (9)0.019 (4)*0.2993
C211/1f0.1220 (9)0.6491 (9)0.6040 (7)0.019 (4)*0.2993
C211/2f0.2414 (9)0.5276 (9)0.6175 (8)0.019 (4)*0.2993
Si21g0.4343 (7)0.7217 (7)0.5385 (7)0.064 (5)*0.566
C211g0.5285 (8)0.8293 (10)0.4979 (7)0.019 (4)*0.7352
C211/1g0.4779 (8)0.6432 (8)0.6086 (8)0.019 (4)*0.7352
C211/2g0.3745 (8)0.6488 (9)0.4418 (8)0.019 (4)*0.7352
Si21h0.4453 (8)0.8344 (7)0.7234 (7)0.064 (5)*
C211h0.3923 (9)0.8525 (8)0.8284 (8)0.019 (4)*
C211/1h0.5048 (8)0.7470 (9)0.7434 (8)0.019 (4)*
C211/2h0.5261 (9)0.9546 (9)0.6865 (8)0.019 (4)*
Geometric parameters (Å, º) top
Si0a—C11a1.973 (19)C11e—C111/2e1.714 (18)
Si0a—C11b1.973 (17)C11f—C111f1.71 (2)
Si0a—C11c1.973 (15)C11f—C111/1f1.71 (2)
Si0a—C11d1.973 (18)C11f—C111/2f1.714 (16)
Si0a—Si21a2.376 (19)C11g—C111g1.714 (15)
Si0a—Si21c2.376 (16)C11g—C111/1g1.714 (19)
Si0a—Si21d2.38 (2)C11g—C111/2g1.714 (18)
C11a—C111a1.714 (19)Si21a—C211a1.97 (2)
C11a—C111/1a1.714 (18)Si21a—C211/1a1.965 (17)
C11a—C111/2a1.714 (19)Si21a—C211/2a1.965 (18)
C11b—C111b1.71 (2)Si21c—C211c1.97 (2)
C11b—C111/1b1.71 (2)Si21c—C211/1c1.97 (2)
C11b—C111/2b1.714 (18)Si21c—C211/2c1.97 (2)
C11c—C111c1.714 (19)Si21d—C211d1.97 (2)
C11c—C111/1c1.714 (19)Si21d—C211/1d1.965 (18)
C11c—C111/2c1.71 (2)Si21d—C211/2d1.965 (16)
C11d—C111d1.71 (2)Si21e—C211e1.965 (16)
C11d—C111/1d1.714 (19)Si21e—C211/1e1.965 (17)
C11d—C111/2d1.714 (16)Si21e—C211/2e1.965 (18)
Si0e—C11e1.973 (19)Si21f—C211f1.965 (18)
Si0e—C11f1.973 (14)Si21f—C211/1f1.97 (2)
Si0e—C11g1.973 (17)Si21f—C211/2f1.97 (2)
Si0e—Si21e2.376 (19)Si21g—C211g1.965 (15)
Si0e—Si21f2.376 (14)Si21g—C211/1g1.965 (19)
Si0e—Si21g2.376 (18)Si21g—C211/2g1.965 (17)
Si0e—Si21h2.376 (15)Si21h—C211h1.965 (19)
C11e—C111e1.714 (16)Si21h—C211/1h1.97 (2)
C11e—C111/1e1.714 (16)Si21h—C211/2h1.965 (15)
C11a—Si0a—C11b123.6 (9)Si21f—Si0e—Si21g107.9 (6)
C11a—Si0a—C11c76.8 (7)Si21f—Si0e—Si21h116.4 (6)
C11a—Si0a—C11d85.3 (7)Si21g—Si0e—Si21h90.9 (6)
C11a—Si0a—Si21a13.8 (4)Si0e—C11e—C111e110.9 (9)
C11a—Si0a—Si21c88.7 (6)Si0e—C11e—C111/1e110.9 (8)
C11a—Si0a—Si21d119.5 (7)Si0e—C11e—C111/2e110.9 (8)
C11b—Si0a—C11c116.0 (7)C111e—C11e—C111/1e108.0 (8)
C11b—Si0a—C11d119.7 (7)C111e—C11e—C111/2e108.0 (8)
C11b—Si0a—Si21a121.4 (8)C111/1e—C11e—C111/2e108.0 (10)
C11b—Si0a—Si21c119.9 (7)Si0e—C11f—C111f110.9 (8)
C11b—Si0a—Si21d101.6 (7)Si0e—C11f—C111/1f110.9 (8)
C11c—Si0a—C11d122.1 (8)Si0e—C11f—C111/2f110.9 (8)
C11c—Si0a—Si21a89.9 (6)C111f—C11f—C111/1f108.0 (9)
C11c—Si0a—Si21c17.6 (6)C111f—C11f—C111/2f108.0 (9)
C11c—Si0a—Si21d119.6 (8)C111/1f—C11f—C111/2f108.0 (9)
C11d—Si0a—Si21a74.5 (6)Si0e—C11g—C111g110.9 (8)
C11d—Si0a—Si21c111.3 (7)Si0e—C11g—C111/1g110.9 (8)
C11d—Si0a—Si21d35.0 (6)Si0e—C11g—C111/2g110.9 (9)
Si21a—Si0a—Si21c100.5 (6)C111g—C11g—C111/1g108.0 (10)
Si21a—Si0a—Si21d109.4 (6)C111g—C11g—C111/2g108.0 (8)
Si21c—Si0a—Si21d102.5 (7)C111/1g—C11g—C111/2g108.0 (9)
Si0a—C11a—C111a110.9 (9)Si0a—Si21a—C211a109.8 (8)
Si0a—C11a—C111/1a110.9 (8)Si0a—Si21a—C211/1a109.8 (7)
Si0a—C11a—C111/2a110.9 (10)Si0a—Si21a—C211/2a109.8 (8)
C111a—C11a—C111/1a108.0 (11)C211a—Si21a—C211/1a109.2 (9)
C111a—C11a—C111/2a108.0 (9)C211a—Si21a—C211/2a109.2 (8)
C111/1a—C11a—C111/2a108.0 (9)C211/1a—Si21a—C211/2a109.2 (8)
Si0a—C11b—C111b110.9 (8)Si0a—Si21c—C211c109.8 (7)
Si0a—C11b—C111/1b110.9 (10)Si0a—Si21c—C211/1c109.8 (7)
Si0a—C11b—C111/2b110.9 (9)Si0a—Si21c—C211/2c109.8 (9)
C111b—C11b—C111/1b108.0 (10)C211c—Si21c—C211/1c109.2 (10)
C111b—C11b—C111/2b108.0 (11)C211c—Si21c—C211/2c109.2 (8)
C111/1b—C11b—C111/2b108.0 (9)C211/1c—Si21c—C211/2c109.2 (8)
Si0a—C11c—C111c110.9 (9)Si0a—Si21d—C211d109.8 (7)
Si0a—C11c—C111/1c110.9 (9)Si0a—Si21d—C211/1d109.8 (8)
Si0a—C11c—C111/2c110.9 (9)Si0a—Si21d—C211/2d109.8 (8)
C111c—C11c—C111/1c108.0 (10)C211d—Si21d—C211/1d109.2 (9)
C111c—C11c—C111/2c108.0 (10)C211d—Si21d—C211/2d109.2 (9)
C111/1c—C11c—C111/2c108.0 (10)C211/1d—Si21d—C211/2d109.2 (8)
Si0a—C11d—C111d110.9 (8)Si0e—Si21e—C211e109.8 (8)
Si0a—C11d—C111/1d110.9 (10)Si0e—Si21e—C211/1e109.8 (7)
Si0a—C11d—C111/2d110.9 (9)Si0e—Si21e—C211/2e109.8 (7)
C111d—C11d—C111/1d108.0 (9)C211e—Si21e—C211/1e109.2 (7)
C111d—C11d—C111/2d108.0 (10)C211e—Si21e—C211/2e109.2 (8)
C111/1d—C11d—C111/2d108.0 (9)C211/1e—Si21e—C211/2e109.2 (8)
C11e—Si0e—C11f118.6 (8)Si0e—Si21f—C211f109.8 (6)
C11e—Si0e—C11g98.9 (7)Si0e—Si21f—C211/1f109.8 (7)
C11e—Si0e—Si21e22.0 (4)Si0e—Si21f—C211/2f109.8 (7)
C11e—Si0e—Si21f108.6 (7)C211f—Si21f—C211/1f109.2 (8)
C11e—Si0e—Si21g117.6 (6)C211f—Si21f—C211/2f109.2 (8)
C11e—Si0e—Si21h114.6 (6)C211/1f—Si21f—C211/2f109.2 (8)
C11f—Si0e—C11g119.9 (7)Si0e—Si21g—C211g109.8 (7)
C11f—Si0e—Si21e98.6 (7)Si0e—Si21g—C211/1g109.8 (7)
C11f—Si0e—Si21f19.7 (4)Si0e—Si21g—C211/2g109.8 (8)
C11f—Si0e—Si21g112.7 (7)C211g—Si21g—C211/1g109.2 (8)
C11f—Si0e—Si21h96.9 (6)C211g—Si21g—C211/2g109.2 (7)
C11g—Si0e—Si21e119.0 (7)C211/1g—Si21g—C211/2g109.2 (8)
C11g—Si0e—Si21f108.1 (6)Si0e—Si21h—C211h109.8 (7)
C11g—Si0e—Si21g21.1 (5)Si0e—Si21h—C211/1h109.8 (7)
C11g—Si0e—Si21h108.6 (7)Si0e—Si21h—C211/2h109.8 (7)
Si21e—Si0e—Si21f92.6 (6)C211h—Si21h—C211/1h109.2 (8)
Si21e—Si0e—Si21g138.9 (6)C211h—Si21h—C211/2h109.2 (7)
Si21e—Si0e—Si21h111.7 (6)C211/1h—Si21h—C211/2h109.2 (8)
(2at295) top
Crystal data top
C13H36Si4Dx = 0.878 (1) Mg m3
Mr = 304.8Synchrotron radiation, λ = 0.399828(2) Å
Cubic, Fm3mµ = 0.19 mm1
a = 13.2645 (2) ÅT = 295 K
V = 2333.9 (1) Å3colourless
Z = 4cylinder, 0.5 × 0.5 mm
F(000) = 680
Data collection top
Two-circle
diffractometer
Data collection mode: transmission
Radiation source: synchrotron, ESRF beamline BM16Scan method: continuous
Si(111) monochromator2θmin = 1.12°, 2θmax = 21.52°, 2θstep = 0.005°
Specimen mounting: lithiumborate glass capillary 0.5 mm diameter
Refinement top
Refinement on Inet13 parameters
Rp = 0.1970 restraints
Rwp = 0.268Only H-atom displacement parameters refined
Rexp = 0.240Weighting scheme based on measured s.u.'s
R(F) = 0.501Background function: Manual background combined with 4 Legendre polynoms
4081 data pointsPreferred orientation correction: none
Profile function: Lorentzian
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si00000.230 (18)*
Si10001.14 (14)*
C10001.14 (14)*
Met10000.98 (7)*
Met20000.98 (7)*
H10000.98 (7)*
H20000.98 (7)*
 

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