Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807000360/bt2233sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807000360/bt2233Isup2.hkl |
CCDC reference: 636165
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
(C16H36N)[FeSi7ClO12(C4H9)7] | F(000) = 4856 |
Mr = 1122.17 | Dx = 1.196 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 8154 reflections |
a = 23.6451 (11) Å | θ = 2.2–30.0° |
b = 32.1149 (15) Å | µ = 0.47 mm−1 |
c = 18.3528 (9) Å | T = 150 K |
β = 116.586 (1)° | Block, yellow |
V = 12462.8 (10) Å3 | 0.36 × 0.28 × 0.14 mm |
Z = 8 |
Bruker SMART APEX CCD diffractometer | 12260 independent reflections |
Radiation source: fine-focus sealed tube | 8887 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
ω scans | θmax = 26.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −29→29 |
Tmin = 0.849, Tmax = 0.937 | k = −39→39 |
54262 measured reflections | l = −22→22 |
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)] = 0.067 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.170 | H-atom parameters constrained |
S = 1.29 | w = 1/[σ2(Fo2) + (0.078P)2] where P = (Fo2 + 2Fc2)/3 |
12260 reflections | (Δ/σ)max = 0.011 |
595 parameters | Δρmax = 1.06 e Å−3 |
0 restraints | Δρmin = −0.39 e Å−3 |
Experimental. IR [KBr, \n (cm-1)]: 2953 (vs), 2872 (s), 1477 (m), 1466 (m), 1402 (w), 1383(w), 1365(w), 1331 (w), 1230 (m), 1170 (s), 1101(vs), 1035(s), 939 (s), 835 (m), 738 (m), 470 (s). Analysis calculated for C44H99FeClNO12Si7: C 47.09, H 8.89, N 1.25%; found: C 46.87, H 9.17, N 1.32%. |
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 | ||
Fe | 0.81780 (2) | 0.067978 (15) | 0.29531 (3) | 0.03476 (15) | |
Cl | 0.89193 (4) | 0.01816 (3) | 0.32439 (6) | 0.0471 (2) | |
Si1 | 0.80387 (4) | 0.14999 (3) | 0.18230 (6) | 0.0323 (2) | |
Si2 | 0.66048 (5) | 0.13932 (4) | 0.09519 (6) | 0.0411 (3) | |
Si3 | 0.64464 (5) | 0.19551 (3) | 0.22278 (6) | 0.0358 (2) | |
Si4 | 0.65241 (4) | 0.11514 (3) | 0.32700 (6) | 0.0351 (2) | |
Si5 | 0.79642 (4) | 0.12701 (3) | 0.42399 (5) | 0.0313 (2) | |
Si6 | 0.66679 (5) | 0.05883 (3) | 0.19917 (6) | 0.0412 (3) | |
Si7 | 0.78663 (4) | 0.20513 (3) | 0.31330 (5) | 0.0303 (2) | |
O1 | 0.82846 (12) | 0.10636 (7) | 0.22764 (15) | 0.0423 (6) | |
O2 | 0.73251 (12) | 0.14612 (9) | 0.10870 (14) | 0.0484 (7) | |
O3 | 0.64127 (12) | 0.17641 (9) | 0.13948 (15) | 0.0471 (7) | |
O4 | 0.63902 (11) | 0.15815 (8) | 0.27761 (15) | 0.0454 (6) | |
O5 | 0.72278 (11) | 0.11668 (7) | 0.40158 (13) | 0.0379 (6) | |
O6 | 0.82626 (11) | 0.09050 (8) | 0.39236 (14) | 0.0421 (6) | |
O7 | 0.73938 (12) | 0.04430 (8) | 0.24068 (17) | 0.0487 (7) | |
O8 | 0.65606 (12) | 0.09535 (9) | 0.13426 (16) | 0.0530 (7) | |
O9 | 0.79843 (11) | 0.17079 (8) | 0.38206 (14) | 0.0424 (6) | |
O10 | 0.71223 (11) | 0.21848 (7) | 0.27195 (14) | 0.0399 (6) | |
O11 | 0.80275 (11) | 0.18543 (7) | 0.24413 (13) | 0.0383 (6) | |
O12 | 0.64778 (12) | 0.07694 (8) | 0.26745 (15) | 0.0486 (7) | |
C1 | 0.85801 (18) | 0.17004 (12) | 0.1427 (2) | 0.0446 (9) | |
H1A | 0.9003 | 0.1733 | 0.1895 | 0.054* | |
H1B | 0.8618 | 0.1485 | 0.1066 | 0.054* | |
C2 | 0.8411 (2) | 0.21106 (14) | 0.0958 (3) | 0.0674 (13) | |
H2A | 0.8181 | 0.2289 | 0.1186 | 0.081* | |
C3 | 0.7978 (3) | 0.20295 (18) | 0.0077 (3) | 0.0915 (18) | |
H3A | 0.7862 | 0.2294 | −0.0219 | 0.137* | |
H3B | 0.7595 | 0.1889 | 0.0029 | 0.137* | |
H3C | 0.8193 | 0.1852 | −0.0156 | 0.137* | |
C4 | 0.9004 (4) | 0.2341 (2) | 0.1058 (4) | 0.124 (3) | |
H4A | 0.8885 | 0.2606 | 0.0762 | 0.186* | |
H4B | 0.9236 | 0.2170 | 0.0837 | 0.186* | |
H4C | 0.9274 | 0.2395 | 0.1637 | 0.186* | |
C5 | 0.60607 (18) | 0.14124 (14) | −0.0145 (2) | 0.0518 (10) | |
H5A | 0.5648 | 0.1298 | −0.0225 | 0.062* | |
H5B | 0.5991 | 0.1708 | −0.0313 | 0.062* | |
C6 | 0.6261 (2) | 0.11837 (16) | −0.0718 (2) | 0.0605 (12) | |
H6A | 0.6682 | 0.1296 | −0.0627 | 0.073* | |
C7 | 0.5793 (3) | 0.1271 (2) | −0.1602 (3) | 0.0959 (19) | |
H7A | 0.5758 | 0.1573 | −0.1696 | 0.144* | |
H7B | 0.5377 | 0.1158 | −0.1711 | 0.144* | |
H7C | 0.5942 | 0.1139 | −0.1965 | 0.144* | |
C8 | 0.6337 (3) | 0.07215 (18) | −0.0543 (3) | 0.0841 (17) | |
H8A | 0.6640 | 0.0676 | 0.0028 | 0.126* | |
H8B | 0.6491 | 0.0587 | −0.0899 | 0.126* | |
H8C | 0.5927 | 0.0601 | −0.0644 | 0.126* | |
C9 | 0.57889 (17) | 0.23212 (12) | 0.2007 (2) | 0.0451 (9) | |
H9A | 0.5431 | 0.2161 | 0.2005 | 0.054* | |
H9B | 0.5925 | 0.2521 | 0.2465 | 0.054* | |
C10 | 0.5538 (2) | 0.25734 (14) | 0.1216 (3) | 0.0572 (11) | |
H10A | 0.5399 | 0.2371 | 0.0754 | 0.069* | |
C11 | 0.6033 (2) | 0.28458 (18) | 0.1172 (3) | 0.0799 (16) | |
H11A | 0.6393 | 0.2675 | 0.1227 | 0.120* | |
H11B | 0.6174 | 0.3051 | 0.1615 | 0.120* | |
H11C | 0.5857 | 0.2991 | 0.0647 | 0.120* | |
C12 | 0.4957 (2) | 0.28238 (17) | 0.1115 (4) | 0.0902 (18) | |
H12A | 0.4796 | 0.2982 | 0.0605 | 0.135* | |
H12B | 0.5075 | 0.3017 | 0.1574 | 0.135* | |
H12C | 0.4629 | 0.2634 | 0.1102 | 0.135* | |
C13 | 0.59168 (17) | 0.10727 (12) | 0.3626 (2) | 0.0444 (9) | |
H13A | 0.5547 | 0.0940 | 0.3177 | 0.053* | |
H13B | 0.6087 | 0.0870 | 0.4080 | 0.053* | |
C14 | 0.5681 (2) | 0.14421 (15) | 0.3909 (3) | 0.0680 (13) | |
H14A | 0.5457 | 0.1617 | 0.3410 | 0.082* | |
C15 | 0.6155 (3) | 0.17173 (19) | 0.4494 (4) | 0.098 (2) | |
H15A | 0.6467 | 0.1790 | 0.4301 | 0.148* | |
H15B | 0.6367 | 0.1576 | 0.5022 | 0.148* | |
H15C | 0.5950 | 0.1972 | 0.4554 | 0.148* | |
C16 | 0.5172 (2) | 0.13231 (17) | 0.4165 (3) | 0.0738 (14) | |
H16A | 0.5031 | 0.1573 | 0.4345 | 0.111* | |
H16B | 0.5345 | 0.1122 | 0.4614 | 0.111* | |
H16C | 0.4812 | 0.1198 | 0.3702 | 0.111* | |
C17 | 0.84048 (17) | 0.13345 (11) | 0.53571 (19) | 0.0369 (8) | |
H17A | 0.8478 | 0.1054 | 0.5609 | 0.044* | |
H17B | 0.8824 | 0.1454 | 0.5482 | 0.044* | |
C18 | 0.80981 (18) | 0.16067 (12) | 0.5770 (2) | 0.0450 (9) | |
H18A | 0.7658 | 0.1502 | 0.5595 | 0.054* | |
C19 | 0.8054 (2) | 0.20575 (14) | 0.5536 (3) | 0.0696 (13) | |
H19A | 0.7816 | 0.2084 | 0.4943 | 0.104* | |
H19B | 0.8481 | 0.2171 | 0.5715 | 0.104* | |
H19C | 0.7837 | 0.2212 | 0.5798 | 0.104* | |
C20 | 0.8453 (3) | 0.15651 (17) | 0.6694 (3) | 0.0835 (16) | |
H20A | 0.8248 | 0.1739 | 0.6946 | 0.125* | |
H20B | 0.8891 | 0.1656 | 0.6881 | 0.125* | |
H20C | 0.8447 | 0.1274 | 0.6848 | 0.125* | |
C21 | 0.6125 (3) | 0.01651 (16) | 0.1409 (3) | 0.0783 (16) | |
H21A | 0.5706 | 0.0296 | 0.1089 | 0.094* | |
H21B | 0.6270 | 0.0066 | 0.1010 | 0.094* | |
C22 | 0.6022 (4) | −0.0185 (2) | 0.1767 (4) | 0.119 (2) | |
H22A | 0.6432 | −0.0313 | 0.2158 | 0.143* | |
C23 | 0.5601 (4) | −0.0515 (2) | 0.1097 (6) | 0.170 (4) | |
H23A | 0.5780 | −0.0562 | 0.0714 | 0.256* | |
H23B | 0.5169 | −0.0409 | 0.0801 | 0.256* | |
H23C | 0.5595 | −0.0779 | 0.1363 | 0.256* | |
C24 | 0.5615 (6) | −0.0070 (3) | 0.2204 (7) | 0.270 (8) | |
H24A | 0.5832 | 0.0146 | 0.2613 | 0.405* | |
H24B | 0.5552 | −0.0317 | 0.2472 | 0.405* | |
H24C | 0.5204 | 0.0036 | 0.1805 | 0.405* | |
C25 | 0.83946 (18) | 0.24976 (12) | 0.3605 (2) | 0.0434 (9) | |
H25A | 0.8180 | 0.2687 | 0.3828 | 0.052* | |
H25B | 0.8780 | 0.2392 | 0.4072 | 0.052* | |
C26 | 0.8601 (2) | 0.27529 (15) | 0.3070 (3) | 0.0650 (13) | |
H26A | 0.8765 | 0.2551 | 0.2794 | 0.078* | |
C27 | 0.9138 (3) | 0.3048 (2) | 0.3554 (4) | 0.127 (3) | |
H27A | 0.9253 | 0.3205 | 0.3182 | 0.191* | |
H27B | 0.9505 | 0.2888 | 0.3935 | 0.191* | |
H27C | 0.9005 | 0.3242 | 0.3859 | 0.191* | |
C28 | 0.8067 (3) | 0.2975 (2) | 0.2419 (4) | 0.121 (3) | |
H28A | 0.7731 | 0.2776 | 0.2107 | 0.182* | |
H28B | 0.8213 | 0.3111 | 0.2055 | 0.182* | |
H28C | 0.7904 | 0.3185 | 0.2661 | 0.182* | |
N | 0.87882 (14) | 0.02840 (10) | 0.05273 (17) | 0.0416 (7) | |
C29 | 0.83980 (19) | 0.04428 (13) | −0.0331 (2) | 0.0540 (11) | |
H29A | 0.8689 | 0.0505 | −0.0572 | 0.065* | |
H29B | 0.8116 | 0.0215 | −0.0656 | 0.065* | |
C30 | 0.7998 (2) | 0.08234 (14) | −0.0425 (3) | 0.0584 (11) | |
H30A | 0.8274 | 0.1063 | −0.0146 | 0.070* | |
H30B | 0.7715 | 0.0773 | −0.0168 | 0.070* | |
C31 | 0.7605 (3) | 0.0925 (2) | −0.1320 (3) | 0.096 (2) | |
H31A | 0.7309 | 0.0691 | −0.1573 | 0.115* | |
H31B | 0.7346 | 0.1173 | −0.1356 | 0.115* | |
C32 | 0.7920 (4) | 0.1001 (3) | −0.1787 (4) | 0.158 (4) | |
H32A | 0.7611 | 0.1057 | −0.2351 | 0.236* | |
H32B | 0.8172 | 0.0756 | −0.1773 | 0.236* | |
H32C | 0.8199 | 0.1242 | −0.1567 | 0.236* | |
C33 | 0.8373 (2) | 0.01577 (13) | 0.0925 (3) | 0.0538 (11) | |
H33A | 0.8648 | 0.0038 | 0.1466 | 0.065* | |
H33B | 0.8178 | 0.0412 | 0.1017 | 0.065* | |
C34 | 0.7854 (2) | −0.01497 (14) | 0.0465 (3) | 0.0698 (13) | |
H34A | 0.8018 | −0.0379 | 0.0252 | 0.084* | |
H34B | 0.7505 | −0.0011 | −0.0001 | 0.084* | |
C35 | 0.7602 (3) | −0.0330 (2) | 0.1079 (4) | 0.106 (2) | |
H35A | 0.7946 | −0.0488 | 0.1518 | 0.127* | |
H35B | 0.7484 | −0.0096 | 0.1334 | 0.127* | |
C36 | 0.7076 (3) | −0.0592 (2) | 0.0680 (5) | 0.133 (3) | |
H36A | 0.6929 | −0.0691 | 0.1071 | 0.199* | |
H36B | 0.7196 | −0.0831 | 0.0447 | 0.199* | |
H36C | 0.6736 | −0.0437 | 0.0243 | 0.199* | |
C37 | 0.91541 (18) | −0.00811 (11) | 0.0440 (2) | 0.0431 (9) | |
H37A | 0.8849 | −0.0270 | 0.0021 | 0.052* | |
H37B | 0.9443 | 0.0025 | 0.0224 | 0.052* | |
C38 | 0.95395 (17) | −0.03370 (11) | 0.1182 (2) | 0.0391 (8) | |
H38A | 0.9258 | −0.0479 | 0.1372 | 0.047* | |
H38B | 0.9832 | −0.0155 | 0.1626 | 0.047* | |
C39 | 0.99108 (18) | −0.06563 (11) | 0.0968 (2) | 0.0441 (9) | |
H39A | 0.9612 | −0.0829 | 0.0510 | 0.053* | |
H39B | 1.0189 | −0.0510 | 0.0779 | 0.053* | |
C40 | 1.0310 (2) | −0.09383 (14) | 0.1666 (3) | 0.0686 (13) | |
H40A | 1.0538 | −0.1136 | 0.1486 | 0.103* | |
H40B | 1.0037 | −0.1091 | 0.1847 | 0.103* | |
H40C | 1.0615 | −0.0771 | 0.2118 | 0.103* | |
C41 | 0.92316 (18) | 0.06185 (11) | 0.1074 (2) | 0.0443 (9) | |
H41A | 0.8974 | 0.0825 | 0.1193 | 0.053* | |
H41B | 0.9519 | 0.0487 | 0.1597 | 0.053* | |
C42 | 0.96273 (18) | 0.08474 (13) | 0.0758 (2) | 0.0510 (10) | |
H42A | 0.9348 | 0.0992 | 0.0246 | 0.061* | |
H42B | 0.9890 | 0.0646 | 0.0636 | 0.061* | |
C43 | 1.00501 (19) | 0.11618 (13) | 0.1371 (3) | 0.0511 (10) | |
H43A | 1.0376 | 0.1012 | 0.1844 | 0.061* | |
H43B | 0.9794 | 0.1328 | 0.1569 | 0.061* | |
C44 | 1.0373 (2) | 0.14524 (16) | 0.1026 (3) | 0.0710 (13) | |
H44A | 1.0655 | 0.1640 | 0.1456 | 0.107* | |
H44B | 1.0054 | 0.1616 | 0.0582 | 0.107* | |
H44C | 1.0620 | 0.1289 | 0.0818 | 0.107* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe | 0.0404 (3) | 0.0268 (3) | 0.0408 (3) | 0.0051 (2) | 0.0215 (2) | −0.0007 (2) |
Cl | 0.0503 (6) | 0.0370 (5) | 0.0559 (6) | 0.0144 (4) | 0.0255 (5) | 0.0029 (4) |
Si1 | 0.0329 (5) | 0.0340 (5) | 0.0334 (5) | 0.0024 (4) | 0.0177 (4) | −0.0005 (4) |
Si2 | 0.0329 (5) | 0.0573 (7) | 0.0313 (5) | 0.0032 (5) | 0.0129 (4) | −0.0067 (5) |
Si3 | 0.0329 (5) | 0.0397 (6) | 0.0353 (5) | 0.0074 (4) | 0.0158 (4) | 0.0009 (4) |
Si4 | 0.0346 (5) | 0.0360 (5) | 0.0394 (5) | −0.0036 (4) | 0.0209 (5) | −0.0054 (4) |
Si5 | 0.0336 (5) | 0.0310 (5) | 0.0295 (5) | 0.0025 (4) | 0.0143 (4) | 0.0010 (4) |
Si6 | 0.0388 (6) | 0.0392 (6) | 0.0493 (6) | −0.0096 (4) | 0.0231 (5) | −0.0155 (5) |
Si7 | 0.0330 (5) | 0.0274 (5) | 0.0313 (5) | 0.0004 (4) | 0.0152 (4) | 0.0000 (4) |
O1 | 0.0490 (15) | 0.0338 (13) | 0.0490 (14) | 0.0025 (11) | 0.0264 (13) | 0.0052 (11) |
O2 | 0.0413 (15) | 0.0696 (19) | 0.0359 (13) | 0.0003 (13) | 0.0188 (12) | −0.0074 (13) |
O3 | 0.0405 (15) | 0.0594 (17) | 0.0418 (14) | 0.0062 (12) | 0.0189 (12) | −0.0072 (12) |
O4 | 0.0434 (15) | 0.0493 (16) | 0.0469 (14) | −0.0005 (12) | 0.0231 (13) | 0.0009 (12) |
O5 | 0.0393 (14) | 0.0417 (14) | 0.0366 (13) | −0.0024 (11) | 0.0206 (11) | −0.0009 (11) |
O6 | 0.0450 (15) | 0.0404 (14) | 0.0419 (14) | 0.0051 (11) | 0.0203 (12) | −0.0074 (11) |
O7 | 0.0440 (15) | 0.0357 (14) | 0.0667 (17) | −0.0036 (11) | 0.0249 (14) | −0.0115 (13) |
O8 | 0.0500 (16) | 0.0601 (18) | 0.0475 (15) | −0.0021 (13) | 0.0206 (13) | −0.0078 (14) |
O9 | 0.0452 (15) | 0.0424 (15) | 0.0374 (13) | −0.0030 (12) | 0.0165 (12) | 0.0087 (11) |
O10 | 0.0353 (13) | 0.0368 (14) | 0.0459 (14) | 0.0062 (11) | 0.0164 (12) | 0.0011 (11) |
O11 | 0.0408 (14) | 0.0394 (14) | 0.0366 (13) | 0.0008 (11) | 0.0190 (12) | −0.0039 (11) |
O12 | 0.0494 (16) | 0.0520 (16) | 0.0513 (15) | −0.0094 (12) | 0.0286 (14) | −0.0196 (13) |
C1 | 0.048 (2) | 0.044 (2) | 0.056 (2) | 0.0041 (18) | 0.036 (2) | 0.0018 (18) |
C2 | 0.101 (4) | 0.053 (3) | 0.078 (3) | 0.013 (3) | 0.067 (3) | 0.012 (2) |
C3 | 0.129 (5) | 0.088 (4) | 0.072 (3) | 0.036 (4) | 0.058 (4) | 0.033 (3) |
C4 | 0.182 (7) | 0.085 (5) | 0.147 (6) | −0.051 (5) | 0.110 (6) | −0.001 (4) |
C5 | 0.040 (2) | 0.073 (3) | 0.037 (2) | 0.003 (2) | 0.0114 (18) | −0.003 (2) |
C6 | 0.051 (3) | 0.092 (4) | 0.037 (2) | −0.008 (2) | 0.019 (2) | −0.012 (2) |
C7 | 0.098 (4) | 0.138 (5) | 0.037 (3) | −0.008 (4) | 0.018 (3) | −0.019 (3) |
C8 | 0.078 (4) | 0.112 (5) | 0.060 (3) | 0.013 (3) | 0.029 (3) | −0.023 (3) |
C9 | 0.040 (2) | 0.048 (2) | 0.050 (2) | 0.0128 (17) | 0.0224 (19) | 0.0030 (18) |
C10 | 0.055 (3) | 0.055 (3) | 0.056 (3) | 0.020 (2) | 0.019 (2) | 0.007 (2) |
C11 | 0.086 (4) | 0.093 (4) | 0.072 (3) | 0.018 (3) | 0.046 (3) | 0.034 (3) |
C12 | 0.065 (3) | 0.084 (4) | 0.113 (4) | 0.033 (3) | 0.032 (3) | 0.030 (3) |
C13 | 0.037 (2) | 0.047 (2) | 0.055 (2) | −0.0043 (17) | 0.0257 (19) | 0.0004 (19) |
C14 | 0.065 (3) | 0.070 (3) | 0.090 (3) | −0.008 (2) | 0.054 (3) | −0.016 (3) |
C15 | 0.088 (4) | 0.106 (5) | 0.129 (5) | −0.024 (3) | 0.074 (4) | −0.059 (4) |
C16 | 0.066 (3) | 0.088 (4) | 0.091 (4) | −0.001 (3) | 0.057 (3) | −0.004 (3) |
C17 | 0.042 (2) | 0.0330 (19) | 0.0314 (17) | 0.0044 (15) | 0.0122 (16) | 0.0039 (15) |
C18 | 0.046 (2) | 0.052 (2) | 0.0349 (19) | 0.0018 (18) | 0.0161 (18) | −0.0046 (17) |
C19 | 0.096 (4) | 0.051 (3) | 0.070 (3) | 0.021 (3) | 0.045 (3) | −0.001 (2) |
C20 | 0.112 (4) | 0.091 (4) | 0.041 (2) | 0.010 (3) | 0.029 (3) | −0.011 (3) |
C21 | 0.096 (4) | 0.067 (3) | 0.102 (4) | −0.041 (3) | 0.071 (3) | −0.049 (3) |
C22 | 0.164 (7) | 0.072 (4) | 0.127 (6) | −0.030 (4) | 0.071 (5) | −0.016 (4) |
C23 | 0.190 (8) | 0.119 (6) | 0.261 (11) | −0.109 (6) | 0.154 (8) | −0.116 (7) |
C24 | 0.48 (2) | 0.186 (10) | 0.343 (15) | −0.208 (12) | 0.364 (16) | −0.170 (10) |
C25 | 0.048 (2) | 0.041 (2) | 0.043 (2) | −0.0098 (17) | 0.0221 (19) | −0.0089 (17) |
C26 | 0.079 (3) | 0.055 (3) | 0.061 (3) | −0.022 (2) | 0.031 (3) | 0.001 (2) |
C27 | 0.155 (7) | 0.136 (6) | 0.109 (5) | −0.101 (5) | 0.076 (5) | −0.031 (4) |
C28 | 0.122 (5) | 0.087 (4) | 0.139 (6) | −0.005 (4) | 0.044 (5) | 0.065 (4) |
N | 0.0477 (18) | 0.0421 (18) | 0.0389 (16) | 0.0040 (14) | 0.0229 (15) | −0.0052 (14) |
C29 | 0.050 (2) | 0.060 (3) | 0.044 (2) | 0.009 (2) | 0.015 (2) | −0.007 (2) |
C30 | 0.057 (3) | 0.061 (3) | 0.055 (2) | 0.018 (2) | 0.024 (2) | 0.007 (2) |
C31 | 0.102 (4) | 0.116 (5) | 0.072 (3) | 0.054 (4) | 0.042 (3) | 0.031 (3) |
C32 | 0.197 (8) | 0.190 (9) | 0.124 (6) | 0.123 (7) | 0.106 (6) | 0.092 (6) |
C33 | 0.064 (3) | 0.043 (2) | 0.071 (3) | 0.006 (2) | 0.046 (2) | −0.005 (2) |
C34 | 0.071 (3) | 0.052 (3) | 0.099 (4) | 0.000 (2) | 0.049 (3) | −0.016 (3) |
C35 | 0.099 (4) | 0.098 (4) | 0.164 (6) | −0.045 (4) | 0.097 (5) | −0.079 (4) |
C36 | 0.134 (6) | 0.123 (6) | 0.181 (7) | −0.030 (5) | 0.106 (6) | −0.069 (6) |
C37 | 0.051 (2) | 0.044 (2) | 0.0393 (19) | 0.0045 (18) | 0.0245 (18) | −0.0055 (17) |
C38 | 0.042 (2) | 0.039 (2) | 0.0404 (19) | −0.0030 (16) | 0.0218 (17) | −0.0062 (16) |
C39 | 0.047 (2) | 0.036 (2) | 0.054 (2) | −0.0019 (17) | 0.026 (2) | −0.0046 (17) |
C40 | 0.080 (3) | 0.050 (3) | 0.083 (3) | 0.016 (2) | 0.043 (3) | 0.006 (2) |
C41 | 0.055 (2) | 0.039 (2) | 0.039 (2) | 0.0059 (18) | 0.0210 (19) | −0.0032 (16) |
C42 | 0.042 (2) | 0.062 (3) | 0.046 (2) | 0.0056 (19) | 0.0165 (19) | 0.003 (2) |
C43 | 0.046 (2) | 0.050 (2) | 0.058 (2) | 0.0039 (19) | 0.024 (2) | −0.003 (2) |
C44 | 0.052 (3) | 0.074 (3) | 0.079 (3) | −0.002 (2) | 0.022 (3) | 0.011 (3) |
Fe—O7 | 1.832 (2) | C18—C20 | 1.524 (5) |
Fe—O1 | 1.846 (2) | C18—H18A | 1.0000 |
Fe—O6 | 1.848 (2) | C19—H19A | 0.9800 |
Fe—Cl | 2.2537 (10) | C19—H19B | 0.9800 |
Si1—O1 | 1.600 (2) | C19—H19C | 0.9800 |
Si1—O11 | 1.616 (2) | C20—H20A | 0.9800 |
Si1—O2 | 1.627 (3) | C20—H20B | 0.9800 |
Si1—C1 | 1.848 (4) | C20—H20C | 0.9800 |
Si2—O8 | 1.608 (3) | C21—C22 | 1.379 (8) |
Si2—O3 | 1.617 (3) | C21—H21A | 0.9900 |
Si2—O2 | 1.622 (3) | C21—H21B | 0.9900 |
Si2—C5 | 1.842 (4) | C22—C24 | 1.549 (11) |
Si3—O4 | 1.609 (3) | C22—C23 | 1.590 (8) |
Si3—O3 | 1.616 (3) | C22—H22A | 1.0000 |
Si3—O10 | 1.619 (3) | C23—H23A | 0.9800 |
Si3—C9 | 1.844 (4) | C23—H23B | 0.9800 |
Si4—O4 | 1.604 (3) | C23—H23C | 0.9800 |
Si4—O5 | 1.614 (2) | C24—H24A | 0.9800 |
Si4—O12 | 1.614 (3) | C24—H24B | 0.9800 |
Si4—C13 | 1.842 (4) | C24—H24C | 0.9800 |
Si5—O6 | 1.605 (2) | C25—C26 | 1.518 (5) |
Si5—O9 | 1.614 (2) | C25—H25A | 0.9900 |
Si5—O5 | 1.634 (2) | C25—H25B | 0.9900 |
Si5—C17 | 1.849 (3) | C26—C28 | 1.476 (7) |
Si6—O7 | 1.604 (3) | C26—C27 | 1.514 (7) |
Si6—O8 | 1.609 (3) | C26—H26A | 1.0000 |
Si6—O12 | 1.617 (3) | C27—H27A | 0.9800 |
Si6—C21 | 1.847 (4) | C27—H27B | 0.9800 |
Si7—O9 | 1.604 (2) | C27—H27C | 0.9800 |
Si7—O11 | 1.609 (2) | C28—H28A | 0.9800 |
Si7—O10 | 1.631 (2) | C28—H28B | 0.9800 |
Si7—C25 | 1.843 (4) | C28—H28C | 0.9800 |
C1—C2 | 1.526 (6) | N—C37 | 1.508 (4) |
C1—H1A | 0.9900 | N—C29 | 1.515 (5) |
C1—H1B | 0.9900 | N—C33 | 1.516 (5) |
C2—C3 | 1.500 (7) | N—C41 | 1.523 (5) |
C2—C4 | 1.523 (7) | C29—C30 | 1.508 (6) |
C2—H2A | 1.0000 | C29—H29A | 0.9900 |
C3—H3A | 0.9800 | C29—H29B | 0.9900 |
C3—H3B | 0.9800 | C30—C31 | 1.517 (6) |
C3—H3C | 0.9800 | C30—H30A | 0.9900 |
C4—H4A | 0.9800 | C30—H30B | 0.9900 |
C4—H4B | 0.9800 | C31—C32 | 1.385 (8) |
C4—H4C | 0.9800 | C31—H31A | 0.9900 |
C5—C6 | 1.521 (5) | C31—H31B | 0.9900 |
C5—H5A | 0.9900 | C32—H32A | 0.9800 |
C5—H5B | 0.9900 | C32—H32B | 0.9800 |
C6—C8 | 1.513 (7) | C32—H32C | 0.9800 |
C6—C7 | 1.526 (6) | C33—C34 | 1.506 (6) |
C6—H6A | 1.0000 | C33—H33A | 0.9900 |
C7—H7A | 0.9800 | C33—H33B | 0.9900 |
C7—H7B | 0.9800 | C34—C35 | 1.600 (8) |
C7—H7C | 0.9800 | C34—H34A | 0.9900 |
C8—H8A | 0.9800 | C34—H34B | 0.9900 |
C8—H8B | 0.9800 | C35—C36 | 1.405 (8) |
C8—H8C | 0.9800 | C35—H35A | 0.9900 |
C9—C10 | 1.530 (5) | C35—H35B | 0.9900 |
C9—H9A | 0.9900 | C36—H36A | 0.9800 |
C9—H9B | 0.9900 | C36—H36B | 0.9800 |
C10—C11 | 1.493 (7) | C36—H36C | 0.9800 |
C10—C12 | 1.528 (6) | C37—C38 | 1.500 (5) |
C10—H10A | 1.0000 | C37—H37A | 0.9900 |
C11—H11A | 0.9800 | C37—H37B | 0.9900 |
C11—H11B | 0.9800 | C38—C39 | 1.512 (5) |
C11—H11C | 0.9800 | C38—H38A | 0.9900 |
C12—H12A | 0.9800 | C38—H38B | 0.9900 |
C12—H12B | 0.9800 | C39—C40 | 1.507 (6) |
C12—H12C | 0.9800 | C39—H39A | 0.9900 |
C13—C14 | 1.499 (6) | C39—H39B | 0.9900 |
C13—H13A | 0.9900 | C40—H40A | 0.9800 |
C13—H13B | 0.9900 | C40—H40B | 0.9800 |
C14—C15 | 1.453 (7) | C40—H40C | 0.9800 |
C14—C16 | 1.525 (6) | C41—C42 | 1.495 (5) |
C14—H14A | 1.0000 | C41—H41A | 0.9900 |
C15—H15A | 0.9800 | C41—H41B | 0.9900 |
C15—H15B | 0.9800 | C42—C43 | 1.509 (5) |
C15—H15C | 0.9800 | C42—H42A | 0.9900 |
C16—H16A | 0.9800 | C42—H42B | 0.9900 |
C16—H16B | 0.9800 | C43—C44 | 1.512 (6) |
C16—H16C | 0.9800 | C43—H43A | 0.9900 |
C17—C18 | 1.535 (5) | C43—H43B | 0.9900 |
C17—H17A | 0.9900 | C44—H44A | 0.9800 |
C17—H17B | 0.9900 | C44—H44B | 0.9800 |
C18—C19 | 1.500 (6) | C44—H44C | 0.9800 |
O7—Fe—O1 | 108.57 (12) | C19—C18—H18A | 107.7 |
O7—Fe—O6 | 109.65 (11) | C20—C18—H18A | 107.7 |
O1—Fe—O6 | 113.50 (11) | C17—C18—H18A | 107.7 |
O7—Fe—Cl | 108.93 (8) | C18—C19—H19A | 109.5 |
O1—Fe—Cl | 107.91 (8) | C18—C19—H19B | 109.5 |
O6—Fe—Cl | 108.19 (8) | H19A—C19—H19B | 109.5 |
O1—Si1—O11 | 111.60 (13) | C18—C19—H19C | 109.5 |
O1—Si1—O2 | 111.43 (14) | H19A—C19—H19C | 109.5 |
O11—Si1—O2 | 107.46 (13) | H19B—C19—H19C | 109.5 |
O1—Si1—C1 | 110.79 (16) | C18—C20—H20A | 109.5 |
O11—Si1—C1 | 105.22 (16) | C18—C20—H20B | 109.5 |
O2—Si1—C1 | 110.11 (16) | H20A—C20—H20B | 109.5 |
O8—Si2—O3 | 109.49 (14) | C18—C20—H20C | 109.5 |
O8—Si2—O2 | 108.86 (15) | H20A—C20—H20C | 109.5 |
O3—Si2—O2 | 109.62 (14) | H20B—C20—H20C | 109.5 |
O8—Si2—C5 | 111.33 (18) | C22—C21—Si6 | 123.4 (5) |
O3—Si2—C5 | 107.99 (17) | C22—C21—H21A | 106.5 |
O2—Si2—C5 | 109.53 (16) | Si6—C21—H21A | 106.5 |
O4—Si3—O3 | 109.02 (14) | C22—C21—H21B | 106.5 |
O4—Si3—O10 | 109.17 (13) | Si6—C21—H21B | 106.5 |
O3—Si3—O10 | 108.59 (14) | H21A—C21—H21B | 106.5 |
O4—Si3—C9 | 108.39 (16) | C21—C22—C24 | 109.5 (7) |
O3—Si3—C9 | 110.75 (16) | C21—C22—C23 | 111.0 (6) |
O10—Si3—C9 | 110.89 (16) | C24—C22—C23 | 104.0 (7) |
O4—Si4—O5 | 108.70 (13) | C21—C22—H22A | 110.7 |
O4—Si4—O12 | 109.60 (14) | C24—C22—H22A | 110.7 |
O5—Si4—O12 | 109.22 (14) | C23—C22—H22A | 110.7 |
O4—Si4—C13 | 109.31 (16) | C22—C23—H23A | 109.5 |
O5—Si4—C13 | 112.01 (15) | C22—C23—H23B | 109.5 |
O12—Si4—C13 | 107.97 (16) | H23A—C23—H23B | 109.5 |
O6—Si5—O9 | 110.64 (13) | C22—C23—H23C | 109.5 |
O6—Si5—O5 | 110.61 (13) | H23A—C23—H23C | 109.5 |
O9—Si5—O5 | 108.20 (13) | H23B—C23—H23C | 109.5 |
O6—Si5—C17 | 111.21 (14) | C22—C24—H24A | 109.5 |
O9—Si5—C17 | 108.01 (15) | C22—C24—H24B | 109.5 |
O5—Si5—C17 | 108.06 (14) | H24A—C24—H24B | 109.5 |
O7—Si6—O8 | 110.14 (15) | C22—C24—H24C | 109.5 |
O7—Si6—O12 | 110.24 (14) | H24A—C24—H24C | 109.5 |
O8—Si6—O12 | 107.78 (15) | H24B—C24—H24C | 109.5 |
O7—Si6—C21 | 112.3 (2) | C26—C25—Si7 | 117.5 (3) |
O8—Si6—C21 | 105.6 (2) | C26—C25—H25A | 107.9 |
O12—Si6—C21 | 110.56 (18) | Si7—C25—H25A | 107.9 |
O9—Si7—O11 | 109.35 (13) | C26—C25—H25B | 107.9 |
O9—Si7—O10 | 108.57 (13) | Si7—C25—H25B | 107.9 |
O11—Si7—O10 | 108.86 (13) | H25A—C25—H25B | 107.2 |
O9—Si7—C25 | 108.80 (15) | C28—C26—C27 | 111.2 (5) |
O11—Si7—C25 | 109.06 (15) | C28—C26—C25 | 112.3 (4) |
O10—Si7—C25 | 112.16 (16) | C27—C26—C25 | 112.7 (4) |
Si1—O1—Fe | 143.84 (16) | C28—C26—H26A | 106.7 |
Si2—O2—Si1 | 139.90 (16) | C27—C26—H26A | 106.7 |
Si3—O3—Si2 | 148.10 (18) | C25—C26—H26A | 106.7 |
Si4—O4—Si3 | 160.86 (18) | C26—C27—H27A | 109.5 |
Si4—O5—Si5 | 142.90 (15) | C26—C27—H27B | 109.5 |
Si5—O6—Fe | 139.36 (15) | H27A—C27—H27B | 109.5 |
Si6—O7—Fe | 138.14 (16) | C26—C27—H27C | 109.5 |
Si2—O8—Si6 | 161.81 (19) | H27A—C27—H27C | 109.5 |
Si7—O9—Si5 | 160.49 (17) | H27B—C27—H27C | 109.5 |
Si3—O10—Si7 | 136.84 (16) | C26—C28—H28A | 109.5 |
Si7—O11—Si1 | 156.20 (17) | C26—C28—H28B | 109.5 |
Si4—O12—Si6 | 147.15 (18) | H28A—C28—H28B | 109.5 |
C2—C1—Si1 | 118.0 (3) | C26—C28—H28C | 109.5 |
C2—C1—H1A | 107.8 | H28A—C28—H28C | 109.5 |
Si1—C1—H1A | 107.8 | H28B—C28—H28C | 109.5 |
C2—C1—H1B | 107.8 | C37—N—C29 | 105.2 (3) |
Si1—C1—H1B | 107.8 | C37—N—C33 | 111.7 (3) |
H1A—C1—H1B | 107.1 | C29—N—C33 | 111.5 (3) |
C3—C2—C4 | 111.2 (5) | C37—N—C41 | 111.1 (3) |
C3—C2—C1 | 109.8 (4) | C29—N—C41 | 111.5 (3) |
C4—C2—C1 | 110.9 (4) | C33—N—C41 | 105.9 (3) |
C3—C2—H2A | 108.3 | C30—C29—N | 116.8 (3) |
C4—C2—H2A | 108.3 | C30—C29—H29A | 108.1 |
C1—C2—H2A | 108.3 | N—C29—H29A | 108.1 |
C2—C3—H3A | 109.5 | C30—C29—H29B | 108.1 |
C2—C3—H3B | 109.5 | N—C29—H29B | 108.1 |
H3A—C3—H3B | 109.5 | H29A—C29—H29B | 107.3 |
C2—C3—H3C | 109.5 | C29—C30—C31 | 110.3 (4) |
H3A—C3—H3C | 109.5 | C29—C30—H30A | 109.6 |
H3B—C3—H3C | 109.5 | C31—C30—H30A | 109.6 |
C2—C4—H4A | 109.5 | C29—C30—H30B | 109.6 |
C2—C4—H4B | 109.5 | C31—C30—H30B | 109.6 |
H4A—C4—H4B | 109.5 | H30A—C30—H30B | 108.1 |
C2—C4—H4C | 109.5 | C32—C31—C30 | 118.0 (6) |
H4A—C4—H4C | 109.5 | C32—C31—H31A | 107.8 |
H4B—C4—H4C | 109.5 | C30—C31—H31A | 107.8 |
C6—C5—Si2 | 117.3 (3) | C32—C31—H31B | 107.8 |
C6—C5—H5A | 108.0 | C30—C31—H31B | 107.8 |
Si2—C5—H5A | 108.0 | H31A—C31—H31B | 107.1 |
C6—C5—H5B | 108.0 | C31—C32—H32A | 109.5 |
Si2—C5—H5B | 108.0 | C31—C32—H32B | 109.5 |
H5A—C5—H5B | 107.2 | H32A—C32—H32B | 109.5 |
C8—C6—C5 | 111.8 (4) | C31—C32—H32C | 109.5 |
C8—C6—C7 | 111.5 (4) | H32A—C32—H32C | 109.5 |
C5—C6—C7 | 110.1 (4) | H32B—C32—H32C | 109.5 |
C8—C6—H6A | 107.8 | C34—C33—N | 116.5 (3) |
C5—C6—H6A | 107.8 | C34—C33—H33A | 108.2 |
C7—C6—H6A | 107.8 | N—C33—H33A | 108.2 |
C6—C7—H7A | 109.5 | C34—C33—H33B | 108.2 |
C6—C7—H7B | 109.5 | N—C33—H33B | 108.2 |
H7A—C7—H7B | 109.5 | H33A—C33—H33B | 107.3 |
C6—C7—H7C | 109.5 | C33—C34—C35 | 108.1 (4) |
H7A—C7—H7C | 109.5 | C33—C34—H34A | 110.1 |
H7B—C7—H7C | 109.5 | C35—C34—H34A | 110.1 |
C6—C8—H8A | 109.5 | C33—C34—H34B | 110.1 |
C6—C8—H8B | 109.5 | C35—C34—H34B | 110.1 |
H8A—C8—H8B | 109.5 | H34A—C34—H34B | 108.4 |
C6—C8—H8C | 109.5 | C36—C35—C34 | 111.8 (6) |
H8A—C8—H8C | 109.5 | C36—C35—H35A | 109.3 |
H8B—C8—H8C | 109.5 | C34—C35—H35A | 109.3 |
C10—C9—Si3 | 118.5 (3) | C36—C35—H35B | 109.3 |
C10—C9—H9A | 107.7 | C34—C35—H35B | 109.3 |
Si3—C9—H9A | 107.7 | H35A—C35—H35B | 107.9 |
C10—C9—H9B | 107.7 | C35—C36—H36A | 109.5 |
Si3—C9—H9B | 107.7 | C35—C36—H36B | 109.5 |
H9A—C9—H9B | 107.1 | H36A—C36—H36B | 109.5 |
C11—C10—C12 | 111.6 (4) | C35—C36—H36C | 109.5 |
C11—C10—C9 | 112.3 (4) | H36A—C36—H36C | 109.5 |
C12—C10—C9 | 109.9 (4) | H36B—C36—H36C | 109.5 |
C11—C10—H10A | 107.6 | C38—C37—N | 118.2 (3) |
C12—C10—H10A | 107.6 | C38—C37—H37A | 107.7 |
C9—C10—H10A | 107.6 | N—C37—H37A | 107.7 |
C10—C11—H11A | 109.5 | C38—C37—H37B | 107.7 |
C10—C11—H11B | 109.5 | N—C37—H37B | 107.7 |
H11A—C11—H11B | 109.5 | H37A—C37—H37B | 107.1 |
C10—C11—H11C | 109.5 | C37—C38—C39 | 108.8 (3) |
H11A—C11—H11C | 109.5 | C37—C38—H38A | 109.9 |
H11B—C11—H11C | 109.5 | C39—C38—H38A | 109.9 |
C10—C12—H12A | 109.5 | C37—C38—H38B | 109.9 |
C10—C12—H12B | 109.5 | C39—C38—H38B | 109.9 |
H12A—C12—H12B | 109.5 | H38A—C38—H38B | 108.3 |
C10—C12—H12C | 109.5 | C40—C39—C38 | 113.7 (3) |
H12A—C12—H12C | 109.5 | C40—C39—H39A | 108.8 |
H12B—C12—H12C | 109.5 | C38—C39—H39A | 108.8 |
C14—C13—Si4 | 118.9 (3) | C40—C39—H39B | 108.8 |
C14—C13—H13A | 107.6 | C38—C39—H39B | 108.8 |
Si4—C13—H13A | 107.6 | H39A—C39—H39B | 107.7 |
C14—C13—H13B | 107.6 | C39—C40—H40A | 109.5 |
Si4—C13—H13B | 107.6 | C39—C40—H40B | 109.5 |
H13A—C13—H13B | 107.0 | H40A—C40—H40B | 109.5 |
C15—C14—C13 | 117.0 (4) | C39—C40—H40C | 109.5 |
C15—C14—C16 | 112.3 (4) | H40A—C40—H40C | 109.5 |
C13—C14—C16 | 112.1 (4) | H40B—C40—H40C | 109.5 |
C15—C14—H14A | 104.7 | C42—C41—N | 117.2 (3) |
C13—C14—H14A | 104.7 | C42—C41—H41A | 108.0 |
C16—C14—H14A | 104.7 | N—C41—H41A | 108.0 |
C14—C15—H15A | 109.5 | C42—C41—H41B | 108.0 |
C14—C15—H15B | 109.5 | N—C41—H41B | 108.0 |
H15A—C15—H15B | 109.5 | H41A—C41—H41B | 107.2 |
C14—C15—H15C | 109.5 | C41—C42—C43 | 111.2 (3) |
H15A—C15—H15C | 109.5 | C41—C42—H42A | 109.4 |
H15B—C15—H15C | 109.5 | C43—C42—H42A | 109.4 |
C14—C16—H16A | 109.5 | C41—C42—H42B | 109.4 |
C14—C16—H16B | 109.5 | C43—C42—H42B | 109.4 |
H16A—C16—H16B | 109.5 | H42A—C42—H42B | 108.0 |
C14—C16—H16C | 109.5 | C42—C43—C44 | 113.0 (4) |
H16A—C16—H16C | 109.5 | C42—C43—H43A | 109.0 |
H16B—C16—H16C | 109.5 | C44—C43—H43A | 109.0 |
C18—C17—Si5 | 117.1 (2) | C42—C43—H43B | 109.0 |
C18—C17—H17A | 108.0 | C44—C43—H43B | 109.0 |
Si5—C17—H17A | 108.0 | H43A—C43—H43B | 107.8 |
C18—C17—H17B | 108.0 | C43—C44—H44A | 109.5 |
Si5—C17—H17B | 108.0 | C43—C44—H44B | 109.5 |
H17A—C17—H17B | 107.3 | H44A—C44—H44B | 109.5 |
C19—C18—C20 | 109.6 (4) | C43—C44—H44C | 109.5 |
C19—C18—C17 | 113.3 (3) | H44A—C44—H44C | 109.5 |
C20—C18—C17 | 110.7 (3) | H44B—C44—H44C | 109.5 |