Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807011038/ng2229sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807011038/ng2229Isup2.hkl |
CCDC reference: 643069
Data collection: CrysAlis CCD (Oxford Diffraction, 2005); cell refinement: CrysAlis RED (Oxford Diffraction, 2005); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Cr(C12H27O4Si)2(C4H8O)2] | F(000) = 1078 |
Mr = 986.49 | Dx = 1.159 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 6408 reflections |
a = 13.862 (3) Å | θ = 2.9–32.5° |
b = 16.583 (3) Å | µ = 0.32 mm−1 |
c = 13.959 (3) Å | T = 100 K |
β = 118.27 (3)° | Fragment, green |
V = 2826.1 (13) Å3 | 0.41 × 0.22 × 0.2 mm |
Z = 2 |
Oxford Diffraction KM-4-CCD diffractometer | Rint = 0.035 |
Graphite monochromator | θmax = 27.5°, θmin = 2.9° |
0.75° ω scans | h = −17→18 |
19226 measured reflections | k = −17→21 |
10013 independent reflections | l = −18→18 |
9641 reflections with I > 2σ(I) |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.047 | H-atom parameters constrained |
wR(F2) = 0.12 | w = 1/[σ2(Fo2) + (0.0733P)2 + 1.7977P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.001 |
10013 reflections | Δρmax = 1.27 e Å−3 |
587 parameters | Δρmin = −0.32 e Å−3 |
1 restraint | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.514 (19) |
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 | ||
Cr1 | 0.97145 (3) | 0.04529 (3) | 0.28070 (3) | 0.01181 (9) | |
Si1 | 0.90112 (5) | 0.03022 (4) | 0.01146 (5) | 0.01352 (15) | |
Si2 | 0.73014 (5) | 0.06111 (4) | 0.28206 (5) | 0.01409 (15) | |
Si3 | 1.23104 (6) | 0.06046 (5) | 0.48003 (5) | 0.01754 (16) | |
O1 | 0.93359 (14) | 0.05060 (14) | 0.13398 (13) | 0.0180 (4) | |
O2 | 1.00431 (15) | −0.00355 (13) | −0.00353 (15) | 0.0174 (4) | |
O3 | 0.81281 (16) | −0.04382 (13) | −0.02897 (14) | 0.0178 (4) | |
O4 | 0.85479 (15) | 0.10873 (13) | −0.06868 (15) | 0.0186 (4) | |
O5 | 0.83973 (15) | 0.03170 (13) | 0.28238 (15) | 0.0210 (4) | |
O6 | 0.75272 (16) | 0.09750 (13) | 0.40004 (15) | 0.0198 (4) | |
O7 | 0.67684 (17) | 0.13531 (14) | 0.19579 (17) | 0.0238 (5) | |
O8 | 0.64396 (16) | −0.01306 (14) | 0.25667 (15) | 0.0198 (4) | |
O9 | 1.10175 (17) | 0.04905 (17) | 0.41557 (16) | 0.0306 (5) | |
O10 | 1.3019 (2) | 0.01228 (16) | 0.4356 (2) | 0.0349 (6) | |
O11 | 1.28383 (17) | 0.03454 (17) | 0.60948 (16) | 0.0298 (5) | |
O12 | 1.25334 (17) | 0.15719 (14) | 0.47225 (17) | 0.0251 (5) | |
O13 | 0.99161 (19) | −0.07607 (13) | 0.28750 (16) | 0.0213 (4) | |
O14 | 0.96240 (15) | 0.16627 (13) | 0.28400 (15) | 0.0167 (4) | |
C1 | 1.1033 (2) | 0.0327 (2) | 0.0091 (2) | 0.0233 (6) | |
C2 | 1.1593 (3) | 0.0802 (3) | 0.1151 (4) | 0.0518 (12) | |
H2A | 1.1143 | 0.1271 | 0.1108 | 0.062* | |
H2B | 1.2314 | 0.0985 | 0.1271 | 0.062* | |
H2C | 1.1681 | 0.0457 | 0.1757 | 0.062* | |
C3 | 1.1760 (3) | −0.0367 (3) | 0.0119 (3) | 0.0352 (8) | |
H3A | 1.1939 | −0.0703 | 0.076 | 0.042* | |
H3B | 1.2436 | −0.0154 | 0.0157 | 0.042* | |
H3C | 1.1373 | −0.0693 | −0.0541 | 0.042* | |
C4 | 1.0779 (4) | 0.0863 (3) | −0.0878 (4) | 0.0579 (14) | |
H4A | 1.0453 | 0.0539 | −0.1544 | 0.07* | |
H4B | 1.1456 | 0.1113 | −0.0791 | 0.07* | |
H4C | 1.0262 | 0.1285 | −0.0926 | 0.07* | |
C5 | 0.7785 (3) | −0.09907 (19) | −0.1192 (2) | 0.0222 (6) | |
C6 | 0.8590 (3) | −0.1695 (2) | −0.0851 (3) | 0.0309 (7) | |
H6A | 0.9326 | −0.1492 | −0.0643 | 0.037* | |
H6B | 0.8366 | −0.2072 | −0.146 | 0.037* | |
H6C | 0.8593 | −0.1974 | −0.023 | 0.037* | |
C7 | 0.7727 (3) | −0.0577 (2) | −0.2192 (2) | 0.0260 (6) | |
H7A | 0.7257 | −0.0099 | −0.2366 | 0.031* | |
H7B | 0.7421 | −0.0951 | −0.2809 | 0.031* | |
H7C | 0.8464 | −0.0414 | −0.2043 | 0.031* | |
C8 | 0.6655 (3) | −0.1287 (2) | −0.1425 (3) | 0.0336 (8) | |
H8A | 0.671 | −0.1576 | −0.0789 | 0.04* | |
H8B | 0.6366 | −0.1651 | −0.2053 | 0.04* | |
H8C | 0.6161 | −0.0825 | −0.1584 | 0.04* | |
C9 | 0.7663 (2) | 0.16384 (19) | −0.0928 (2) | 0.0187 (5) | |
C10 | 0.7994 (3) | 0.2246 (2) | −0.0009 (3) | 0.0275 (7) | |
H10A | 0.8105 | 0.1966 | 0.0654 | 0.033* | |
H10B | 0.7415 | 0.265 | −0.0209 | 0.033* | |
H10C | 0.8677 | 0.2513 | 0.0121 | 0.033* | |
C11 | 0.6627 (2) | 0.1199 (2) | −0.1107 (3) | 0.0261 (6) | |
H11A | 0.643 | 0.0797 | −0.1685 | 0.031* | |
H11B | 0.6028 | 0.1588 | −0.132 | 0.031* | |
H11C | 0.6755 | 0.0929 | −0.0432 | 0.031* | |
C12 | 0.7475 (3) | 0.2067 (2) | −0.1969 (3) | 0.0321 (7) | |
H12A | 0.8153 | 0.2335 | −0.1851 | 0.038* | |
H12B | 0.6894 | 0.2471 | −0.2166 | 0.038* | |
H12C | 0.7256 | 0.1673 | −0.2558 | 0.038* | |
C13 | 0.7711 (2) | 0.05784 (19) | 0.49903 (19) | 0.0179 (5) | |
C14 | 0.8362 (3) | −0.0191 (2) | 0.5166 (3) | 0.0291 (7) | |
H14A | 0.7952 | −0.0563 | 0.4562 | 0.035* | |
H14B | 0.8485 | −0.0443 | 0.585 | 0.035* | |
H14C | 0.9068 | −0.0065 | 0.5201 | 0.035* | |
C15 | 0.8353 (3) | 0.1174 (2) | 0.5901 (2) | 0.0302 (7) | |
H15A | 0.9065 | 0.1277 | 0.5936 | 0.036* | |
H15B | 0.8464 | 0.0948 | 0.6594 | 0.036* | |
H15C | 0.7943 | 0.168 | 0.5758 | 0.036* | |
C16 | 0.6602 (2) | 0.0405 (3) | 0.4925 (3) | 0.0372 (8) | |
H16A | 0.6212 | 0.0914 | 0.4849 | 0.045* | |
H16B | 0.671 | 0.0129 | 0.559 | 0.045* | |
H16C | 0.617 | 0.0061 | 0.4294 | 0.045* | |
C17 | 0.5895 (3) | 0.1906 (2) | 0.1791 (3) | 0.0267 (7) | |
C18 | 0.6393 (4) | 0.2618 (3) | 0.2549 (4) | 0.0515 (11) | |
H18A | 0.672 | 0.2433 | 0.3305 | 0.062* | |
H18B | 0.582 | 0.3016 | 0.2418 | 0.062* | |
H18C | 0.6959 | 0.2865 | 0.2414 | 0.062* | |
C19 | 0.5018 (3) | 0.1513 (3) | 0.1990 (3) | 0.0362 (8) | |
H19A | 0.4748 | 0.1026 | 0.1543 | 0.043* | |
H19B | 0.441 | 0.1892 | 0.1796 | 0.043* | |
H19C | 0.5328 | 0.1368 | 0.276 | 0.043* | |
C20 | 0.5402 (4) | 0.2173 (3) | 0.0607 (3) | 0.0519 (13) | |
H20A | 0.598 | 0.2395 | 0.0469 | 0.062* | |
H20B | 0.4845 | 0.2587 | 0.0461 | 0.062* | |
H20C | 0.5064 | 0.1709 | 0.0129 | 0.062* | |
C21 | 0.6017 (2) | −0.0732 (2) | 0.1720 (2) | 0.0210 (6) | |
C22 | 0.6852 (3) | −0.1397 (2) | 0.2007 (3) | 0.0365 (8) | |
H22A | 0.7514 | −0.1183 | 0.2015 | 0.044* | |
H22B | 0.6547 | −0.1829 | 0.1466 | 0.044* | |
H22C | 0.7036 | −0.1613 | 0.2728 | 0.044* | |
C23 | 0.4994 (3) | −0.1058 (3) | 0.1711 (4) | 0.0456 (11) | |
H23A | 0.5183 | −0.1291 | 0.2424 | 0.055* | |
H23B | 0.467 | −0.1476 | 0.1151 | 0.055* | |
H23C | 0.4466 | −0.062 | 0.1552 | 0.055* | |
C24 | 0.5784 (4) | −0.0360 (3) | 0.0631 (3) | 0.0416 (9) | |
H24A | 0.5256 | 0.0082 | 0.0454 | 0.05* | |
H24B | 0.5478 | −0.0772 | 0.0061 | 0.05* | |
H24C | 0.6466 | −0.0151 | 0.0678 | 0.05* | |
C25 | 1.3517 (2) | −0.0678 (2) | 0.4569 (3) | 0.0249 (6) | |
C26 | 1.4571 (3) | −0.0663 (3) | 0.5635 (3) | 0.0367 (8) | |
H26A | 1.5063 | −0.0254 | 0.56 | 0.044* | |
H26B | 1.4923 | −0.1194 | 0.5767 | 0.044* | |
H26C | 1.4408 | −0.0532 | 0.6228 | 0.044* | |
C27 | 1.3732 (3) | −0.0810 (3) | 0.3613 (3) | 0.0389 (9) | |
H27A | 1.304 | −0.0776 | 0.2934 | 0.047* | |
H27B | 1.4059 | −0.1344 | 0.3671 | 0.047* | |
H27C | 1.4237 | −0.0395 | 0.3616 | 0.047* | |
C28 | 1.2735 (3) | −0.1294 (3) | 0.4601 (4) | 0.0451 (10) | |
H28A | 1.2621 | −0.119 | 0.5231 | 0.054* | |
H28B | 1.3041 | −0.1835 | 0.466 | 0.054* | |
H28C | 1.2033 | −0.1256 | 0.3933 | 0.054* | |
C29 | 1.2497 (2) | 0.0462 (2) | 0.6894 (2) | 0.0240 (6) | |
C30 | 1.3518 (3) | 0.0337 (4) | 0.7984 (3) | 0.0575 (14) | |
H30A | 1.3867 | −0.0174 | 0.7973 | 0.069* | |
H30B | 1.3312 | 0.0325 | 0.8566 | 0.069* | |
H30C | 1.4032 | 0.0782 | 0.8115 | 0.069* | |
C31 | 1.2014 (5) | 0.1273 (3) | 0.6846 (4) | 0.0591 (14) | |
H31A | 1.2529 | 0.169 | 0.6878 | 0.071* | |
H31B | 1.1869 | 0.1336 | 0.7464 | 0.071* | |
H31C | 1.1327 | 0.1325 | 0.6166 | 0.071* | |
C32 | 1.1708 (4) | −0.0205 (3) | 0.6806 (4) | 0.0548 (12) | |
H32A | 1.1014 | −0.0134 | 0.6137 | 0.066* | |
H32B | 1.1576 | −0.0182 | 0.7436 | 0.066* | |
H32C | 1.2025 | −0.0729 | 0.6789 | 0.066* | |
C33 | 1.3499 (2) | 0.2006 (2) | 0.4886 (2) | 0.0239 (6) | |
C34 | 1.3227 (3) | 0.2891 (2) | 0.4956 (3) | 0.0325 (7) | |
H34A | 1.2604 | 0.3055 | 0.4266 | 0.039* | |
H34B | 1.3864 | 0.3226 | 0.51 | 0.039* | |
H34C | 1.3041 | 0.2958 | 0.5546 | 0.039* | |
C35 | 1.4502 (3) | 0.1752 (3) | 0.5939 (3) | 0.0460 (11) | |
H35A | 1.4377 | 0.187 | 0.6559 | 0.055* | |
H35B | 1.5145 | 0.2051 | 0.6017 | 0.055* | |
H35C | 1.4628 | 0.1173 | 0.5916 | 0.055* | |
C36 | 1.3698 (3) | 0.1886 (3) | 0.3911 (3) | 0.0357 (8) | |
H36A | 1.3815 | 0.1312 | 0.3835 | 0.043* | |
H36B | 1.4347 | 0.2192 | 0.4022 | 0.043* | |
H36C | 1.306 | 0.2076 | 0.3251 | 0.043* | |
C37 | 0.9874 (2) | −0.11823 (19) | 0.3773 (2) | 0.0198 (6) | |
H37A | 0.9201 | −0.1035 | 0.3812 | 0.024* | |
H37B | 1.0518 | −0.1042 | 0.4473 | 0.024* | |
C38 | 0.9875 (4) | −0.2060 (2) | 0.3540 (3) | 0.0418 (10) | |
H38A | 0.9228 | −0.2326 | 0.3524 | 0.05* | |
H38B | 1.0544 | −0.2319 | 0.4111 | 0.05* | |
C39 | 0.9841 (4) | −0.2135 (2) | 0.2455 (3) | 0.0450 (11) | |
H39A | 1.0536 | −0.2364 | 0.254 | 0.054* | |
H39B | 0.9232 | −0.2491 | 0.197 | 0.054* | |
C40 | 0.9675 (4) | −0.1309 (2) | 0.1994 (3) | 0.0379 (9) | |
H40A | 1.0171 | −0.1211 | 0.1678 | 0.046* | |
H40B | 0.891 | −0.1239 | 0.1416 | 0.046* | |
C41 | 0.9536 (3) | 0.2061 (2) | 0.3734 (3) | 0.0258 (6) | |
H41A | 0.9943 | 0.1754 | 0.4418 | 0.031* | |
H41B | 0.876 | 0.2101 | 0.3568 | 0.031* | |
C42 | 1.0029 (3) | 0.2895 (2) | 0.3841 (3) | 0.0277 (7) | |
H42A | 1.0778 | 0.2919 | 0.4463 | 0.033* | |
H42B | 0.957 | 0.3311 | 0.3938 | 0.033* | |
C43 | 1.0046 (3) | 0.3009 (2) | 0.2756 (3) | 0.0269 (7) | |
H43A | 0.933 | 0.3202 | 0.2179 | 0.032* | |
H43B | 1.0625 | 0.3393 | 0.2833 | 0.032* | |
C44 | 1.0291 (2) | 0.21669 (18) | 0.2519 (2) | 0.0179 (5) | |
H44A | 1.007 | 0.2099 | 0.1737 | 0.021* | |
H44B | 1.1079 | 0.2038 | 0.2954 | 0.021* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr1 | 0.01052 (16) | 0.0145 (2) | 0.01016 (16) | −0.00051 (16) | 0.00467 (13) | −0.00085 (15) |
Si1 | 0.0168 (3) | 0.0138 (4) | 0.0102 (3) | 0.0002 (3) | 0.0066 (2) | 0.0001 (2) |
Si2 | 0.0143 (3) | 0.0143 (4) | 0.0167 (3) | 0.0021 (3) | 0.0097 (2) | 0.0033 (3) |
Si3 | 0.0145 (3) | 0.0163 (4) | 0.0155 (3) | 0.0015 (3) | 0.0019 (2) | 0.0025 (3) |
O1 | 0.0235 (8) | 0.0174 (10) | 0.0127 (7) | −0.0014 (9) | 0.0082 (6) | −0.0029 (8) |
O2 | 0.0187 (9) | 0.0177 (10) | 0.0173 (9) | 0.0020 (7) | 0.0097 (7) | −0.0011 (7) |
O3 | 0.0251 (9) | 0.0173 (10) | 0.0135 (8) | −0.0037 (8) | 0.0111 (8) | −0.0040 (7) |
O4 | 0.0201 (9) | 0.0192 (10) | 0.0178 (8) | 0.0034 (8) | 0.0100 (7) | 0.0055 (8) |
O5 | 0.0194 (8) | 0.0201 (11) | 0.0285 (9) | 0.0011 (8) | 0.0154 (8) | 0.0037 (8) |
O6 | 0.0247 (10) | 0.0172 (10) | 0.0204 (9) | −0.0014 (8) | 0.0131 (8) | 0.0008 (8) |
O7 | 0.0260 (10) | 0.0229 (12) | 0.0270 (10) | 0.0111 (9) | 0.0163 (9) | 0.0099 (8) |
O8 | 0.0205 (9) | 0.0232 (11) | 0.0181 (9) | −0.0054 (8) | 0.0112 (8) | −0.0040 (8) |
O9 | 0.0282 (10) | 0.0256 (12) | 0.0248 (9) | −0.0011 (11) | 0.0017 (8) | −0.0024 (10) |
O10 | 0.0441 (14) | 0.0269 (13) | 0.0384 (13) | 0.0099 (11) | 0.0233 (11) | 0.0048 (10) |
O11 | 0.0272 (10) | 0.0365 (14) | 0.0234 (9) | 0.0040 (10) | 0.0101 (8) | 0.0014 (10) |
O12 | 0.0223 (10) | 0.0198 (11) | 0.0277 (10) | −0.0033 (9) | 0.0072 (8) | −0.0007 (9) |
O13 | 0.0357 (11) | 0.0142 (11) | 0.0186 (10) | 0.0005 (9) | 0.0166 (9) | 0.0008 (7) |
O14 | 0.0186 (9) | 0.0164 (10) | 0.0157 (9) | −0.0033 (7) | 0.0087 (8) | −0.0030 (7) |
C1 | 0.0203 (12) | 0.0261 (17) | 0.0260 (12) | 0.0006 (12) | 0.0131 (10) | 0.0002 (12) |
C2 | 0.0372 (19) | 0.062 (3) | 0.067 (3) | −0.0262 (19) | 0.0335 (19) | −0.040 (2) |
C3 | 0.0282 (16) | 0.040 (2) | 0.0413 (18) | 0.0072 (15) | 0.0197 (15) | −0.0037 (16) |
C4 | 0.044 (2) | 0.074 (4) | 0.073 (3) | 0.021 (2) | 0.042 (2) | 0.047 (3) |
C5 | 0.0299 (15) | 0.0194 (15) | 0.0164 (12) | −0.0068 (12) | 0.0103 (11) | −0.0081 (11) |
C6 | 0.0432 (18) | 0.0216 (17) | 0.0246 (14) | 0.0034 (14) | 0.0133 (14) | −0.0048 (12) |
C7 | 0.0368 (16) | 0.0268 (17) | 0.0140 (12) | −0.0019 (13) | 0.0118 (12) | −0.0063 (11) |
C8 | 0.0378 (18) | 0.0348 (19) | 0.0302 (16) | −0.0160 (15) | 0.0177 (14) | −0.0093 (14) |
C9 | 0.0195 (12) | 0.0181 (14) | 0.0167 (12) | 0.0026 (11) | 0.0073 (10) | 0.0042 (10) |
C10 | 0.0249 (14) | 0.0201 (16) | 0.0274 (14) | 0.0038 (12) | 0.0041 (12) | −0.0017 (12) |
C11 | 0.0183 (12) | 0.0280 (18) | 0.0321 (15) | 0.0010 (12) | 0.0121 (11) | 0.0017 (12) |
C12 | 0.0322 (16) | 0.037 (2) | 0.0282 (15) | 0.0117 (15) | 0.0153 (13) | 0.0195 (14) |
C13 | 0.0184 (11) | 0.0206 (15) | 0.0163 (10) | −0.0002 (11) | 0.0095 (9) | 0.0013 (11) |
C14 | 0.0383 (17) | 0.0228 (16) | 0.0246 (14) | 0.0067 (14) | 0.0136 (13) | 0.0031 (12) |
C15 | 0.0394 (17) | 0.0255 (18) | 0.0249 (14) | −0.0048 (14) | 0.0144 (13) | −0.0047 (12) |
C16 | 0.0279 (14) | 0.058 (3) | 0.0302 (14) | −0.0011 (18) | 0.0172 (12) | 0.0098 (17) |
C17 | 0.0329 (16) | 0.0212 (17) | 0.0269 (15) | 0.0155 (13) | 0.0148 (13) | 0.0118 (12) |
C18 | 0.049 (2) | 0.029 (2) | 0.070 (3) | 0.0106 (18) | 0.023 (2) | −0.006 (2) |
C19 | 0.0297 (16) | 0.037 (2) | 0.048 (2) | 0.0145 (15) | 0.0234 (15) | 0.0095 (16) |
C20 | 0.063 (3) | 0.063 (3) | 0.042 (2) | 0.042 (2) | 0.034 (2) | 0.031 (2) |
C21 | 0.0200 (13) | 0.0225 (16) | 0.0178 (12) | −0.0010 (11) | 0.0069 (11) | −0.0051 (11) |
C22 | 0.0371 (18) | 0.0283 (19) | 0.0344 (17) | 0.0059 (15) | 0.0091 (15) | −0.0065 (14) |
C23 | 0.0324 (18) | 0.059 (3) | 0.049 (2) | −0.0200 (18) | 0.0217 (17) | −0.029 (2) |
C24 | 0.068 (3) | 0.034 (2) | 0.0201 (14) | 0.0044 (18) | 0.0182 (16) | 0.0014 (13) |
C25 | 0.0197 (13) | 0.0243 (17) | 0.0284 (15) | 0.0044 (12) | 0.0095 (12) | −0.0008 (12) |
C26 | 0.0249 (16) | 0.051 (2) | 0.0298 (17) | 0.0045 (16) | 0.0097 (14) | 0.0017 (16) |
C27 | 0.042 (2) | 0.039 (2) | 0.0313 (17) | 0.0006 (17) | 0.0141 (16) | −0.0058 (15) |
C28 | 0.038 (2) | 0.0253 (19) | 0.077 (3) | −0.0028 (16) | 0.031 (2) | −0.0008 (19) |
C29 | 0.0271 (12) | 0.0254 (16) | 0.0214 (11) | 0.0045 (14) | 0.0130 (10) | 0.0019 (13) |
C30 | 0.046 (2) | 0.093 (4) | 0.0267 (16) | 0.006 (3) | 0.0114 (15) | 0.006 (2) |
C31 | 0.105 (4) | 0.038 (3) | 0.048 (2) | 0.028 (3) | 0.048 (3) | 0.0044 (18) |
C32 | 0.056 (3) | 0.057 (3) | 0.065 (3) | −0.019 (2) | 0.040 (2) | −0.016 (2) |
C33 | 0.0191 (13) | 0.0232 (16) | 0.0220 (13) | −0.0059 (12) | 0.0038 (11) | 0.0009 (11) |
C34 | 0.0321 (17) | 0.0252 (18) | 0.0368 (17) | −0.0032 (14) | 0.0136 (14) | 0.0005 (14) |
C35 | 0.0285 (18) | 0.036 (2) | 0.041 (2) | −0.0080 (16) | −0.0104 (15) | 0.0053 (17) |
C36 | 0.0351 (18) | 0.037 (2) | 0.0400 (19) | −0.0010 (15) | 0.0216 (16) | −0.0024 (15) |
C37 | 0.0253 (14) | 0.0205 (15) | 0.0164 (12) | 0.0013 (11) | 0.0122 (11) | 0.0060 (10) |
C38 | 0.078 (3) | 0.0203 (18) | 0.046 (2) | 0.0049 (18) | 0.044 (2) | 0.0071 (15) |
C39 | 0.085 (3) | 0.0204 (18) | 0.0298 (17) | 0.0081 (19) | 0.028 (2) | −0.0010 (14) |
C40 | 0.071 (3) | 0.0194 (17) | 0.0306 (17) | 0.0009 (17) | 0.0295 (18) | −0.0043 (13) |
C41 | 0.0384 (17) | 0.0187 (15) | 0.0309 (15) | −0.0031 (13) | 0.0252 (14) | −0.0068 (12) |
C42 | 0.0380 (17) | 0.0197 (16) | 0.0283 (15) | −0.0059 (13) | 0.0180 (14) | −0.0085 (12) |
C43 | 0.0371 (17) | 0.0141 (15) | 0.0299 (15) | −0.0023 (13) | 0.0161 (13) | −0.0027 (11) |
C44 | 0.0178 (12) | 0.0152 (14) | 0.0188 (12) | −0.0028 (10) | 0.0071 (10) | −0.0012 (10) |
Cr1—O1 | 1.8600 (17) | C17—C20 | 1.525 (4) |
Cr1—O5 | 1.8508 (19) | C18—H18A | 0.98 |
Cr1—O9 | 1.895 (2) | C18—H18B | 0.98 |
Cr1—O13 | 2.028 (2) | C18—H18C | 0.98 |
Cr1—O14 | 2.012 (2) | C19—H19A | 0.98 |
Si1—O1 | 1.5852 (18) | C19—H19B | 0.98 |
Si1—O3 | 1.634 (2) | C19—H19C | 0.98 |
Si1—O4 | 1.637 (2) | C20—H20A | 0.98 |
Si1—O2 | 1.639 (2) | C20—H20B | 0.98 |
Si2—O5 | 1.594 (2) | C20—H20C | 0.98 |
Si2—O8 | 1.632 (2) | C21—C22 | 1.510 (5) |
Si2—O7 | 1.633 (2) | C21—C23 | 1.512 (5) |
Si2—O6 | 1.639 (2) | C21—C24 | 1.527 (4) |
Si3—O9 | 1.591 (2) | C22—H22A | 0.98 |
Si3—O10 | 1.602 (3) | C22—H22B | 0.98 |
Si3—O12 | 1.647 (2) | C22—H22C | 0.98 |
Si3—O11 | 1.653 (2) | C23—H23A | 0.98 |
O2—C1 | 1.431 (3) | C23—H23B | 0.98 |
O3—C5 | 1.444 (3) | C23—H23C | 0.98 |
O4—C9 | 1.436 (3) | C24—H24A | 0.98 |
O6—C13 | 1.440 (3) | C24—H24B | 0.98 |
O7—C17 | 1.446 (4) | C24—H24C | 0.98 |
O8—C21 | 1.441 (3) | C25—C28 | 1.505 (5) |
O10—C25 | 1.461 (4) | C25—C26 | 1.513 (4) |
O11—C29 | 1.416 (3) | C25—C27 | 1.515 (5) |
O12—C33 | 1.439 (4) | C26—H26A | 0.98 |
O13—C40 | 1.436 (4) | C26—H26B | 0.98 |
O13—C37 | 1.461 (3) | C26—H26C | 0.98 |
O14—C44 | 1.465 (3) | C27—H27A | 0.98 |
O14—C41 | 1.467 (3) | C27—H27B | 0.98 |
C1—C4 | 1.514 (5) | C27—H27C | 0.98 |
C1—C3 | 1.518 (5) | C28—H28A | 0.98 |
C1—C2 | 1.525 (5) | C28—H28B | 0.98 |
C2—H2A | 0.98 | C28—H28C | 0.98 |
C2—H2B | 0.98 | C29—C31 | 1.489 (5) |
C2—H2C | 0.98 | C29—C32 | 1.520 (6) |
C3—H3A | 0.98 | C29—C30 | 1.524 (4) |
C3—H3B | 0.98 | C30—H30A | 0.98 |
C3—H3C | 0.98 | C30—H30B | 0.98 |
C4—H4A | 0.98 | C30—H30C | 0.98 |
C4—H4B | 0.98 | C31—H31A | 0.98 |
C4—H4C | 0.98 | C31—H31B | 0.98 |
C5—C7 | 1.522 (4) | C31—H31C | 0.98 |
C5—C8 | 1.523 (5) | C32—H32A | 0.98 |
C5—C6 | 1.527 (5) | C32—H32B | 0.98 |
C6—H6A | 0.98 | C32—H32C | 0.98 |
C6—H6B | 0.98 | C33—C36 | 1.524 (5) |
C6—H6C | 0.98 | C33—C35 | 1.528 (4) |
C7—H7A | 0.98 | C33—C34 | 1.530 (5) |
C7—H7B | 0.98 | C34—H34A | 0.98 |
C7—H7C | 0.98 | C34—H34B | 0.98 |
C8—H8A | 0.98 | C34—H34C | 0.98 |
C8—H8B | 0.98 | C35—H35A | 0.98 |
C8—H8C | 0.98 | C35—H35B | 0.98 |
C9—C11 | 1.523 (4) | C35—H35C | 0.98 |
C9—C10 | 1.522 (4) | C36—H36A | 0.98 |
C9—C12 | 1.524 (4) | C36—H36B | 0.98 |
C10—H10A | 0.98 | C36—H36C | 0.98 |
C10—H10B | 0.98 | C37—C38 | 1.491 (5) |
C10—H10C | 0.98 | C37—H37A | 0.99 |
C11—H11A | 0.98 | C37—H37B | 0.99 |
C11—H11B | 0.98 | C38—C39 | 1.498 (5) |
C11—H11C | 0.98 | C38—H38A | 0.99 |
C12—H12A | 0.98 | C38—H38B | 0.99 |
C12—H12B | 0.98 | C39—C40 | 1.483 (5) |
C12—H12C | 0.98 | C39—H39A | 0.99 |
C13—C14 | 1.514 (4) | C39—H39B | 0.99 |
C13—C15 | 1.520 (4) | C40—H40A | 0.99 |
C13—C16 | 1.524 (4) | C40—H40B | 0.99 |
C14—H14A | 0.98 | C41—C42 | 1.518 (5) |
C14—H14B | 0.98 | C41—H41A | 0.99 |
C14—H14C | 0.98 | C41—H41B | 0.99 |
C15—H15A | 0.98 | C42—C43 | 1.537 (5) |
C15—H15B | 0.98 | C42—H42A | 0.99 |
C15—H15C | 0.98 | C42—H42B | 0.99 |
C16—H16A | 0.98 | C43—C44 | 1.511 (4) |
C16—H16B | 0.98 | C43—H43A | 0.99 |
C16—H16C | 0.98 | C43—H43B | 0.99 |
C17—C19 | 1.517 (5) | C44—H44A | 0.99 |
C17—C18 | 1.516 (6) | C44—H44B | 0.99 |
O5—Cr1—O1 | 104.72 (9) | C17—C19—H19B | 109.5 |
O5—Cr1—O9 | 118.25 (10) | H19A—C19—H19B | 109.5 |
O1—Cr1—O9 | 137.02 (9) | C17—C19—H19C | 109.5 |
O5—Cr1—O14 | 92.78 (9) | H19A—C19—H19C | 109.5 |
O1—Cr1—O14 | 89.41 (9) | H19B—C19—H19C | 109.5 |
O9—Cr1—O14 | 89.13 (10) | C17—C20—H20A | 109.5 |
O5—Cr1—O13 | 89.63 (10) | C17—C20—H20B | 109.5 |
O1—Cr1—O13 | 93.40 (9) | H20A—C20—H20B | 109.5 |
O9—Cr1—O13 | 86.61 (11) | C17—C20—H20C | 109.5 |
O14—Cr1—O13 | 175.71 (8) | H20A—C20—H20C | 109.5 |
O1—Si1—O3 | 108.44 (11) | H20B—C20—H20C | 109.5 |
O1—Si1—O4 | 112.76 (12) | O8—C21—C22 | 109.0 (2) |
O3—Si1—O4 | 111.99 (11) | O8—C21—C23 | 105.7 (3) |
O1—Si1—O2 | 113.05 (10) | C22—C21—C23 | 109.8 (3) |
O3—Si1—O2 | 104.80 (11) | O8—C21—C24 | 110.4 (3) |
O4—Si1—O2 | 105.56 (11) | C22—C21—C24 | 109.5 (3) |
O5—Si2—O8 | 111.64 (12) | C23—C21—C24 | 112.4 (3) |
O5—Si2—O7 | 109.29 (11) | C21—C22—H22A | 109.5 |
O8—Si2—O7 | 112.25 (12) | C21—C22—H22B | 109.5 |
O5—Si2—O6 | 112.45 (11) | H22A—C22—H22B | 109.5 |
O8—Si2—O6 | 105.52 (11) | C21—C22—H22C | 109.5 |
O7—Si2—O6 | 105.54 (12) | H22A—C22—H22C | 109.5 |
O9—Si3—O10 | 117.06 (14) | H22B—C22—H22C | 109.5 |
O9—Si3—O12 | 105.96 (13) | C21—C23—H23A | 109.5 |
O10—Si3—O12 | 106.95 (14) | C21—C23—H23B | 109.5 |
O9—Si3—O11 | 112.59 (12) | H23A—C23—H23B | 109.5 |
O10—Si3—O11 | 104.99 (13) | C21—C23—H23C | 109.5 |
O12—Si3—O11 | 109.00 (13) | H23A—C23—H23C | 109.5 |
Si1—O1—Cr1 | 164.96 (15) | H23B—C23—H23C | 109.5 |
C1—O2—Si1 | 133.2 (2) | C21—C24—H24A | 109.5 |
C5—O3—Si1 | 131.40 (18) | C21—C24—H24B | 109.5 |
C9—O4—Si1 | 132.99 (18) | H24A—C24—H24B | 109.5 |
Si2—O5—Cr1 | 155.18 (15) | C21—C24—H24C | 109.5 |
C13—O6—Si2 | 131.21 (19) | H24A—C24—H24C | 109.5 |
C17—O7—Si2 | 130.38 (19) | H24B—C24—H24C | 109.5 |
C21—O8—Si2 | 132.12 (18) | O10—C25—C28 | 110.2 (3) |
Si3—O9—Cr1 | 148.71 (15) | O10—C25—C26 | 109.2 (3) |
C25—O10—Si3 | 133.8 (2) | C28—C25—C26 | 110.8 (3) |
C29—O11—Si3 | 133.3 (2) | O10—C25—C27 | 102.9 (3) |
C33—O12—Si3 | 131.8 (2) | C28—C25—C27 | 112.0 (3) |
C40—O13—C37 | 110.1 (2) | C26—C25—C27 | 111.6 (3) |
C40—O13—Cr1 | 128.13 (19) | C25—C26—H26A | 109.5 |
C37—O13—Cr1 | 117.03 (17) | C25—C26—H26B | 109.5 |
C44—O14—C41 | 108.8 (2) | H26A—C26—H26B | 109.5 |
C44—O14—Cr1 | 120.44 (16) | C25—C26—H26C | 109.5 |
C41—O14—Cr1 | 119.97 (18) | H26A—C26—H26C | 109.5 |
O2—C1—C4 | 109.4 (3) | H26B—C26—H26C | 109.5 |
O2—C1—C3 | 105.7 (3) | C25—C27—H27A | 109.5 |
C4—C1—C3 | 109.9 (3) | C25—C27—H27B | 109.5 |
O2—C1—C2 | 110.7 (2) | H27A—C27—H27B | 109.5 |
C4—C1—C2 | 111.1 (4) | C25—C27—H27C | 109.5 |
C3—C1—C2 | 109.9 (3) | H27A—C27—H27C | 109.5 |
C1—C2—H2A | 109.5 | H27B—C27—H27C | 109.5 |
C1—C2—H2B | 109.5 | C25—C28—H28A | 109.5 |
H2A—C2—H2B | 109.5 | C25—C28—H28B | 109.5 |
C1—C2—H2C | 109.5 | H28A—C28—H28B | 109.5 |
H2A—C2—H2C | 109.5 | C25—C28—H28C | 109.5 |
H2B—C2—H2C | 109.5 | H28A—C28—H28C | 109.5 |
C1—C3—H3A | 109.5 | H28B—C28—H28C | 109.5 |
C1—C3—H3B | 109.5 | O11—C29—C31 | 113.5 (3) |
H3A—C3—H3B | 109.5 | O11—C29—C32 | 109.5 (3) |
C1—C3—H3C | 109.5 | C31—C29—C32 | 111.2 (4) |
H3A—C3—H3C | 109.5 | O11—C29—C30 | 105.7 (3) |
H3B—C3—H3C | 109.5 | C31—C29—C30 | 110.6 (4) |
C1—C4—H4A | 109.5 | C32—C29—C30 | 105.9 (4) |
C1—C4—H4B | 109.5 | C29—C30—H30A | 109.5 |
H4A—C4—H4B | 109.5 | C29—C30—H30B | 109.5 |
C1—C4—H4C | 109.5 | H30A—C30—H30B | 109.5 |
H4A—C4—H4C | 109.5 | C29—C30—H30C | 109.5 |
H4B—C4—H4C | 109.5 | H30A—C30—H30C | 109.5 |
O3—C5—C7 | 111.5 (2) | H30B—C30—H30C | 109.5 |
O3—C5—C8 | 105.8 (2) | C29—C31—H31A | 109.5 |
C7—C5—C8 | 110.3 (3) | C29—C31—H31B | 109.5 |
O3—C5—C6 | 108.9 (2) | H31A—C31—H31B | 109.5 |
C7—C5—C6 | 110.2 (3) | C29—C31—H31C | 109.5 |
C8—C5—C6 | 110.2 (3) | H31A—C31—H31C | 109.5 |
C5—C6—H6A | 109.5 | H31B—C31—H31C | 109.5 |
C5—C6—H6B | 109.5 | C29—C32—H32A | 109.5 |
H6A—C6—H6B | 109.5 | C29—C32—H32B | 109.5 |
C5—C6—H6C | 109.5 | H32A—C32—H32B | 109.5 |
H6A—C6—H6C | 109.5 | C29—C32—H32C | 109.5 |
H6B—C6—H6C | 109.5 | H32A—C32—H32C | 109.5 |
C5—C7—H7A | 109.5 | H32B—C32—H32C | 109.5 |
C5—C7—H7B | 109.5 | O12—C33—C36 | 109.9 (3) |
H7A—C7—H7B | 109.5 | O12—C33—C35 | 111.7 (3) |
C5—C7—H7C | 109.5 | C36—C33—C35 | 110.8 (3) |
H7A—C7—H7C | 109.5 | O12—C33—C34 | 104.6 (3) |
H7B—C7—H7C | 109.5 | C36—C33—C34 | 109.6 (3) |
C5—C8—H8A | 109.5 | C35—C33—C34 | 110.0 (3) |
C5—C8—H8B | 109.5 | C33—C34—H34A | 109.5 |
H8A—C8—H8B | 109.5 | C33—C34—H34B | 109.5 |
C5—C8—H8C | 109.5 | H34A—C34—H34B | 109.5 |
H8A—C8—H8C | 109.5 | C33—C34—H34C | 109.5 |
H8B—C8—H8C | 109.5 | H34A—C34—H34C | 109.5 |
O4—C9—C11 | 111.6 (3) | H34B—C34—H34C | 109.5 |
O4—C9—C10 | 109.9 (2) | C33—C35—H35A | 109.5 |
C11—C9—C10 | 109.8 (3) | C33—C35—H35B | 109.5 |
O4—C9—C12 | 105.2 (2) | H35A—C35—H35B | 109.5 |
C11—C9—C12 | 110.2 (2) | C33—C35—H35C | 109.5 |
C10—C9—C12 | 110.0 (3) | H35A—C35—H35C | 109.5 |
C9—C10—H10A | 109.5 | H35B—C35—H35C | 109.5 |
C9—C10—H10B | 109.5 | C33—C36—H36A | 109.5 |
H10A—C10—H10B | 109.5 | C33—C36—H36B | 109.5 |
C9—C10—H10C | 109.5 | H36A—C36—H36B | 109.5 |
H10A—C10—H10C | 109.5 | C33—C36—H36C | 109.5 |
H10B—C10—H10C | 109.5 | H36A—C36—H36C | 109.5 |
C9—C11—H11A | 109.5 | H36B—C36—H36C | 109.5 |
C9—C11—H11B | 109.5 | O13—C37—C38 | 106.0 (2) |
H11A—C11—H11B | 109.5 | O13—C37—H37A | 110.5 |
C9—C11—H11C | 109.5 | C38—C37—H37A | 110.5 |
H11A—C11—H11C | 109.5 | O13—C37—H37B | 110.5 |
H11B—C11—H11C | 109.5 | C38—C37—H37B | 110.5 |
C9—C12—H12A | 109.5 | H37A—C37—H37B | 108.7 |
C9—C12—H12B | 109.5 | C37—C38—C39 | 107.3 (3) |
H12A—C12—H12B | 109.5 | C37—C38—H38A | 110.2 |
C9—C12—H12C | 109.5 | C39—C38—H38A | 110.2 |
H12A—C12—H12C | 109.5 | C37—C38—H38B | 110.2 |
H12B—C12—H12C | 109.5 | C39—C38—H38B | 110.2 |
O6—C13—C14 | 111.2 (2) | H38A—C38—H38B | 108.5 |
O6—C13—C15 | 105.8 (2) | C40—C39—C38 | 106.7 (3) |
C14—C13—C15 | 110.1 (2) | C40—C39—H39A | 110.4 |
O6—C13—C16 | 108.3 (2) | C38—C39—H39A | 110.4 |
C14—C13—C16 | 111.0 (3) | C40—C39—H39B | 110.4 |
C15—C13—C16 | 110.3 (3) | C38—C39—H39B | 110.4 |
C13—C14—H14A | 109.5 | H39A—C39—H39B | 108.6 |
C13—C14—H14B | 109.5 | O13—C40—C39 | 106.7 (3) |
H14A—C14—H14B | 109.5 | O13—C40—H40A | 110.4 |
C13—C14—H14C | 109.5 | C39—C40—H40A | 110.4 |
H14A—C14—H14C | 109.5 | O13—C40—H40B | 110.4 |
H14B—C14—H14C | 109.5 | C39—C40—H40B | 110.4 |
C13—C15—H15A | 109.5 | H40A—C40—H40B | 108.6 |
C13—C15—H15B | 109.5 | O14—C41—C42 | 106.2 (2) |
H15A—C15—H15B | 109.5 | O14—C41—H41A | 110.5 |
C13—C15—H15C | 109.5 | C42—C41—H41A | 110.5 |
H15A—C15—H15C | 109.5 | O14—C41—H41B | 110.5 |
H15B—C15—H15C | 109.5 | C42—C41—H41B | 110.5 |
C13—C16—H16A | 109.5 | H41A—C41—H41B | 108.7 |
C13—C16—H16B | 109.5 | C41—C42—C43 | 103.4 (2) |
H16A—C16—H16B | 109.5 | C41—C42—H42A | 111.1 |
C13—C16—H16C | 109.5 | C43—C42—H42A | 111.1 |
H16A—C16—H16C | 109.5 | C41—C42—H42B | 111.1 |
H16B—C16—H16C | 109.5 | C43—C42—H42B | 111.1 |
O7—C17—C19 | 112.4 (3) | H42A—C42—H42B | 109 |
O7—C17—C18 | 108.1 (3) | C44—C43—C42 | 102.3 (3) |
C19—C17—C18 | 110.2 (3) | C44—C43—H43A | 111.3 |
O7—C17—C20 | 105.7 (3) | C42—C43—H43A | 111.3 |
C19—C17—C20 | 109.7 (3) | C44—C43—H43B | 111.3 |
C18—C17—C20 | 110.6 (4) | C42—C43—H43B | 111.3 |
C17—C18—H18A | 109.5 | H43A—C43—H43B | 109.2 |
C17—C18—H18B | 109.5 | O14—C44—C43 | 102.7 (2) |
H18A—C18—H18B | 109.5 | O14—C44—H44A | 111.2 |
C17—C18—H18C | 109.5 | C43—C44—H44A | 111.2 |
H18A—C18—H18C | 109.5 | O14—C44—H44B | 111.2 |
H18B—C18—H18C | 109.5 | C43—C44—H44B | 111.2 |
C17—C19—H19A | 109.5 | H44A—C44—H44B | 109.1 |