Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804004325/su6079sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804004325/su6079Isup2.hkl |
CCDC reference: 238638
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.038
- wR factor = 0.108
- Data-to-parameter ratio = 11.8
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 23.26 Deg.
Alert level B THETM01_ALERT_3_B The value of sine(theta_max)/wavelength is less than 0.575 Calculated sin(theta_max)/wavelength = 0.5556 PLAT023_ALERT_3_B Resolution (too) Low [sin(th)/Lambda < 0.6]..... 23.26 Deg.
Alert level C ABSTM02_ALERT_3_C The ratio of Tmax/Tmin expected RT(exp) is > 1.10 Absorption corrections should be applied. Tmin and Tmax expected: 0.626 0.702 RT(exp) = 1.121 PLAT057_ALERT_3_C Correction for Absorption Required RT(exp) ... 1.12 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe3 - C35 .. 6.65 su PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C28 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Si1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Si2 PLAT480_ALERT_4_C Long H...A H-Bond Reported H12A .. O1 .. 2.80 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H33B .. O4 .. 2.78 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H33A .. O7 .. 2.74 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H25B .. O9 .. 2.77 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H34C .. O11 .. 2.77 Ang. PLAT726_ALERT_1_C H...A Calc 2.78960, Rep 2.80000 Dev... 0.01 Ang. H12A -O1 1.555 2.645 PLAT728_ALERT_1_C D-H..A Calc 152.24, Rep 151.00 Dev... 1.24 Deg. C12 -H12A -O1 1.555 1.555 2.645 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.24 Deg. C4 -C3 -FE2 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.00 Deg. C24 -C23 -FE4 1.555 1.555 1.555 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C20 H17 Fe2 N O6 S Si
1 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1990); software used to prepare material for publication: XP.
[Fe2(C14H17NSSi)(CO)6] | F(000) = 2192 |
Mr = 539.20 | Dx = 1.526 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5103 reflections |
a = 25.4591 (11) Å | θ = 3.4–23.4° |
b = 14.1058 (7) Å | µ = 1.41 mm−1 |
c = 13.2386 (6) Å | T = 293 K |
β = 99.223 (3)° | Block, red |
V = 4692.8 (4) Å3 | 0.34 × 0.30 × 0.25 mm |
Z = 8 |
Nonius KappaCCD area-detector diffractometer | 5103 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 23.3°, θmin = 3.4° |
ω scans | h = −28→27 |
6680 measured reflections | k = −15→0 |
6680 independent reflections | l = 0→14 |
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)] = 0.038 | H-atom parameters constrained |
wR(F2) = 0.108 | w = 1/[σ2(Fo2) + (0.0453P)2 + 0.7589P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.006 |
6680 reflections | Δρmax = 0.29 e Å−3 |
566 parameters | Δρmin = −0.28 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0046 (4) |
Experimental. Spectroscopic data, for (3): 1H NMR (CDCl3): 0.28 (s, 9H), 7.18–7.55 (m, 5H), 7.69 (d, 1H), 7.78 (d, 1H), 8.42 (s, 1H); for (4): 1H NMR (CDCl3): 0.23 (s, 9H), 4.26 (s, 2H), 6.94–7.88 (m, 7H); MS (EI): 539 (M+), 511 (M+ - CO), 483 (M+ - 2 CO), 455 (M+ - 3 CO), 427 (M+ - 4 CO), 399 (M+ - 5 CO), 371 (M+ - 6 CO), 186 (C11H8NS+), 112 (Fe2+), 56 (Fe+), 28 (CO+). |
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 on F2 for ALL reflections except for 16 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factor(obs.) 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 | ||
Fe1 | 0.42391 (2) | 0.14905 (3) | 0.21700 (4) | 0.04550 (17) | |
Fe2 | 0.35204 (2) | 0.16274 (3) | 0.07024 (4) | 0.04668 (17) | |
S1 | 0.44194 (5) | 0.33918 (7) | 0.06043 (9) | 0.0659 (3) | |
C1 | 0.50626 (17) | 0.3043 (4) | 0.0572 (3) | 0.0770 (13) | |
H1 | 0.5336 | 0.3466 | 0.0512 | 0.080* | |
C2 | 0.51331 (16) | 0.2097 (3) | 0.0641 (3) | 0.0693 (12) | |
H2 | 0.5457 | 0.1793 | 0.0632 | 0.080* | |
C3 | 0.46474 (14) | 0.1619 (3) | 0.0728 (3) | 0.0508 (9) | |
C4 | 0.42069 (14) | 0.2228 (2) | 0.0724 (3) | 0.0485 (9) | |
C5 | 0.44978 (14) | 0.0598 (3) | 0.0569 (3) | 0.0543 (9) | |
H5A | 0.4412 | 0.0442 | −0.0153 | 0.080* | |
H5B | 0.4778 | 0.0180 | 0.0893 | 0.080* | |
N1 | 0.40204 (10) | 0.05537 (19) | 0.1082 (2) | 0.0437 (7) | |
C6 | 0.38443 (14) | −0.0417 (2) | 0.1146 (3) | 0.0478 (8) | |
C7 | 0.3569 (2) | −0.0844 (3) | 0.0269 (3) | 0.0733 (13) | |
H7 | 0.3491 | −0.0499 | −0.0335 | 0.080* | |
C8 | 0.3412 (2) | −0.1783 (3) | 0.0297 (3) | 0.0755 (13) | |
H8 | 0.3228 | −0.2052 | −0.0297 | 0.080* | |
C9 | 0.35166 (15) | −0.2339 (3) | 0.1169 (3) | 0.0533 (9) | |
C10 | 0.37830 (18) | −0.1891 (3) | 0.2018 (3) | 0.0711 (12) | |
H10 | 0.3861 | −0.2232 | 0.2624 | 0.080* | |
C11 | 0.39421 (18) | −0.0951 (3) | 0.2014 (3) | 0.0680 (12) | |
H11 | 0.4119 | −0.0680 | 0.2614 | 0.080* | |
Si1 | 0.32964 (5) | −0.36084 (7) | 0.11404 (9) | 0.0578 (3) | |
C12 | 0.35533 (18) | −0.4230 (3) | 0.0082 (3) | 0.0725 (12) | |
H12A | 0.3935 | −0.4255 | 0.0227 | 0.080* | |
H12B | 0.3445 | −0.3893 | −0.0547 | 0.080* | |
H12C | 0.3413 | −0.4862 | 0.0018 | 0.080* | |
C13 | 0.25602 (19) | −0.3658 (4) | 0.0933 (4) | 0.0893 (15) | |
H13A | 0.2445 | −0.4297 | 0.0777 | 0.080* | |
H13B | 0.2420 | −0.3251 | 0.0374 | 0.080* | |
H13C | 0.2433 | −0.3452 | 0.1542 | 0.080* | |
C14 | 0.3556 (2) | −0.4182 (3) | 0.2375 (3) | 0.0898 (15) | |
H14A | 0.3938 | −0.4183 | 0.2476 | 0.080* | |
H14B | 0.3429 | −0.4823 | 0.2370 | 0.080* | |
H14C | 0.3436 | −0.3838 | 0.2921 | 0.080* | |
C15 | 0.47819 (17) | 0.0876 (3) | 0.2926 (3) | 0.0652 (11) | |
O1 | 0.51071 (14) | 0.0487 (2) | 0.3449 (3) | 0.1043 (12) | |
C16 | 0.44039 (17) | 0.2592 (3) | 0.2835 (3) | 0.0607 (10) | |
O2 | 0.45158 (15) | 0.3288 (2) | 0.3236 (3) | 0.0889 (10) | |
C17 | 0.37120 (16) | 0.1274 (3) | 0.2874 (3) | 0.0556 (10) | |
O3 | 0.33929 (13) | 0.1133 (2) | 0.3370 (2) | 0.0813 (9) | |
C18 | 0.29552 (16) | 0.0949 (3) | 0.0976 (3) | 0.0619 (10) | |
O4 | 0.25959 (12) | 0.0524 (3) | 0.1128 (3) | 0.0993 (12) | |
C19 | 0.32022 (17) | 0.2721 (3) | 0.0861 (3) | 0.0649 (11) | |
O5 | 0.30026 (15) | 0.3436 (2) | 0.0979 (3) | 0.1003 (12) | |
C20 | 0.33689 (16) | 0.1593 (3) | −0.0661 (4) | 0.0610 (10) | |
O6 | 0.32874 (15) | 0.1604 (2) | −0.1535 (3) | 0.0930 (11) | |
Fe3 | 0.075344 (19) | 0.14899 (3) | −0.19456 (4) | 0.04322 (16) | |
Fe4 | 0.14615 (2) | 0.14966 (3) | −0.30072 (4) | 0.04856 (17) | |
S2 | 0.06606 (4) | 0.34218 (6) | −0.35836 (9) | 0.0616 (3) | |
C21 | −0.00065 (17) | 0.3196 (3) | −0.3922 (3) | 0.0659 (11) | |
H21 | −0.0259 | 0.3668 | −0.4105 | 0.080* | |
C22 | −0.01290 (16) | 0.2270 (3) | −0.3896 (3) | 0.0611 (10) | |
H22 | −0.0472 | 0.2029 | −0.4066 | 0.080* | |
C23 | 0.03329 (14) | 0.1702 (2) | −0.3577 (3) | 0.0482 (9) | |
C24 | 0.08098 (14) | 0.2218 (2) | −0.3355 (3) | 0.0473 (8) | |
C25 | 0.04149 (14) | 0.0661 (2) | −0.3714 (3) | 0.0491 (9) | |
H25A | 0.0116 | 0.0293 | −0.3561 | 0.080* | |
H25B | 0.0478 | 0.0514 | −0.4401 | 0.080* | |
N2 | 0.09020 (11) | 0.05065 (18) | −0.2937 (2) | 0.0438 (7) | |
C26 | 0.10450 (13) | −0.0483 (2) | −0.2814 (3) | 0.0425 (8) | |
C27 | 0.09766 (19) | −0.1070 (3) | −0.3649 (3) | 0.0736 (13) | |
H27 | 0.0821 | −0.0835 | −0.4283 | 0.080* | |
C28 | 0.11392 (19) | −0.2020 (3) | −0.3557 (3) | 0.0762 (14) | |
H28 | 0.1082 | −0.2404 | −0.4135 | 0.080* | |
C29 | 0.13800 (14) | −0.2406 (2) | −0.2646 (3) | 0.0482 (9) | |
C30 | 0.14318 (16) | −0.1802 (3) | −0.1821 (3) | 0.0577 (10) | |
H30 | 0.1585 | −0.2035 | −0.1184 | 0.080* | |
C31 | 0.12658 (15) | −0.0857 (2) | −0.1890 (3) | 0.0541 (9) | |
H31 | 0.1306 | −0.0481 | −0.1305 | 0.080* | |
Si2 | 0.16371 (4) | −0.36556 (7) | −0.25717 (9) | 0.0544 (3) | |
C32 | 0.23678 (18) | −0.3626 (3) | −0.2142 (4) | 0.0850 (14) | |
H32A | 0.2496 | −0.4259 | −0.1997 | 0.080* | |
H32B | 0.2446 | −0.3246 | −0.1535 | 0.080* | |
H32C | 0.2538 | −0.3357 | −0.2672 | 0.080* | |
C33 | 0.14924 (17) | −0.4204 (3) | −0.3856 (3) | 0.0684 (11) | |
H33A | 0.1122 | −0.4124 | −0.4126 | 0.080* | |
H33B | 0.1576 | −0.4867 | −0.3805 | 0.080* | |
H33C | 0.1704 | −0.3903 | −0.4303 | 0.080* | |
C34 | 0.1313 (2) | −0.4340 (3) | −0.1640 (4) | 0.0893 (15) | |
H34A | 0.0934 | −0.4336 | −0.1854 | 0.080* | |
H34B | 0.1397 | −0.4055 | −0.0975 | 0.080* | |
H34C | 0.1440 | −0.4981 | −0.1611 | 0.080* | |
C35 | 0.02291 (16) | 0.0882 (3) | −0.1467 (3) | 0.0548 (9) | |
O7 | −0.01003 (13) | 0.0500 (2) | −0.1136 (3) | 0.0848 (9) | |
C36 | 0.13094 (16) | 0.1360 (2) | −0.0966 (3) | 0.0540 (9) | |
O8 | 0.16447 (13) | 0.1322 (2) | −0.0263 (2) | 0.0784 (9) | |
C37 | 0.05884 (16) | 0.2592 (3) | −0.1396 (3) | 0.0557 (10) | |
O9 | 0.04692 (14) | 0.3286 (2) | −0.1053 (2) | 0.0806 (9) | |
C38 | 0.20067 (16) | 0.0753 (3) | −0.2402 (3) | 0.0633 (11) | |
O10 | 0.23627 (12) | 0.0320 (2) | −0.2031 (3) | 0.0914 (10) | |
C39 | 0.16060 (17) | 0.1379 (3) | −0.4279 (4) | 0.0624 (10) | |
O11 | 0.16930 (15) | 0.1337 (3) | −0.5100 (3) | 0.0944 (10) | |
C40 | 0.18371 (17) | 0.2555 (3) | −0.2660 (4) | 0.0690 (12) | |
O12 | 0.20615 (16) | 0.3229 (3) | −0.2438 (3) | 0.1111 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0510 (3) | 0.0431 (3) | 0.0424 (3) | 0.0018 (2) | 0.0073 (2) | −0.0009 (2) |
Fe2 | 0.0463 (3) | 0.0451 (3) | 0.0482 (3) | −0.0002 (2) | 0.0063 (2) | 0.0012 (2) |
S1 | 0.0804 (7) | 0.0501 (6) | 0.0639 (7) | −0.0159 (5) | 0.0018 (6) | 0.0079 (5) |
C1 | 0.069 (3) | 0.090 (3) | 0.072 (3) | −0.033 (3) | 0.009 (2) | 0.008 (3) |
C2 | 0.055 (2) | 0.085 (3) | 0.068 (3) | −0.015 (2) | 0.010 (2) | 0.005 (2) |
C3 | 0.049 (2) | 0.055 (2) | 0.049 (2) | −0.0021 (17) | 0.0101 (17) | 0.0015 (17) |
C4 | 0.059 (2) | 0.046 (2) | 0.039 (2) | −0.0085 (17) | 0.0038 (16) | 0.0005 (16) |
C5 | 0.055 (2) | 0.056 (2) | 0.055 (2) | 0.0059 (18) | 0.0180 (18) | −0.0040 (18) |
N1 | 0.0497 (16) | 0.0394 (16) | 0.0443 (16) | −0.0010 (12) | 0.0145 (13) | −0.0011 (13) |
C6 | 0.057 (2) | 0.043 (2) | 0.045 (2) | −0.0023 (16) | 0.0118 (17) | −0.0045 (16) |
C7 | 0.124 (4) | 0.049 (2) | 0.044 (2) | −0.013 (2) | 0.002 (2) | 0.0009 (18) |
C8 | 0.120 (4) | 0.056 (2) | 0.045 (2) | −0.023 (3) | −0.002 (2) | −0.003 (2) |
C9 | 0.067 (2) | 0.049 (2) | 0.046 (2) | −0.0046 (18) | 0.0134 (18) | 0.0024 (17) |
C10 | 0.102 (3) | 0.050 (2) | 0.054 (3) | −0.012 (2) | −0.011 (2) | 0.011 (2) |
C11 | 0.093 (3) | 0.052 (2) | 0.051 (2) | −0.013 (2) | −0.015 (2) | 0.0065 (19) |
Si1 | 0.0715 (7) | 0.0472 (6) | 0.0551 (7) | −0.0108 (5) | 0.0110 (5) | 0.0002 (5) |
C12 | 0.086 (3) | 0.060 (3) | 0.071 (3) | 0.000 (2) | 0.011 (2) | −0.007 (2) |
C13 | 0.087 (3) | 0.086 (4) | 0.098 (4) | −0.021 (3) | 0.026 (3) | −0.004 (3) |
C14 | 0.126 (4) | 0.066 (3) | 0.075 (3) | −0.018 (3) | 0.007 (3) | 0.014 (2) |
C15 | 0.067 (3) | 0.054 (2) | 0.070 (3) | 0.009 (2) | −0.002 (2) | −0.008 (2) |
O1 | 0.098 (2) | 0.088 (2) | 0.109 (3) | 0.029 (2) | −0.037 (2) | −0.007 (2) |
C16 | 0.076 (3) | 0.055 (3) | 0.052 (2) | 0.002 (2) | 0.013 (2) | −0.001 (2) |
O2 | 0.137 (3) | 0.0579 (19) | 0.072 (2) | −0.0182 (18) | 0.019 (2) | −0.0216 (16) |
C17 | 0.064 (2) | 0.058 (2) | 0.046 (2) | 0.0018 (19) | 0.010 (2) | 0.0023 (18) |
O3 | 0.080 (2) | 0.101 (2) | 0.067 (2) | −0.0073 (18) | 0.0286 (17) | 0.0102 (18) |
C18 | 0.052 (2) | 0.071 (3) | 0.063 (3) | 0.001 (2) | 0.008 (2) | 0.010 (2) |
O4 | 0.0618 (19) | 0.111 (3) | 0.128 (3) | −0.0139 (19) | 0.0250 (19) | 0.031 (2) |
C19 | 0.067 (3) | 0.060 (3) | 0.066 (3) | 0.015 (2) | 0.005 (2) | 0.001 (2) |
O5 | 0.106 (3) | 0.077 (2) | 0.117 (3) | 0.036 (2) | 0.015 (2) | −0.001 (2) |
C20 | 0.065 (3) | 0.059 (2) | 0.059 (3) | −0.0127 (19) | 0.009 (2) | 0.008 (2) |
O6 | 0.119 (3) | 0.103 (3) | 0.052 (2) | −0.039 (2) | −0.0011 (19) | 0.0068 (17) |
Fe3 | 0.0502 (3) | 0.0383 (3) | 0.0419 (3) | −0.0012 (2) | 0.0096 (2) | −0.0011 (2) |
Fe4 | 0.0499 (3) | 0.0432 (3) | 0.0546 (3) | −0.0032 (2) | 0.0146 (2) | −0.0016 (2) |
S2 | 0.0779 (7) | 0.0400 (5) | 0.0693 (7) | 0.0030 (5) | 0.0192 (5) | 0.0084 (5) |
C21 | 0.072 (3) | 0.054 (2) | 0.071 (3) | 0.016 (2) | 0.009 (2) | 0.010 (2) |
C22 | 0.061 (2) | 0.053 (2) | 0.067 (3) | 0.0060 (19) | 0.004 (2) | 0.002 (2) |
C23 | 0.060 (2) | 0.0414 (19) | 0.043 (2) | 0.0038 (17) | 0.0094 (17) | 0.0029 (16) |
C24 | 0.058 (2) | 0.0381 (18) | 0.047 (2) | −0.0009 (16) | 0.0144 (17) | −0.0002 (16) |
C25 | 0.055 (2) | 0.046 (2) | 0.043 (2) | 0.0032 (17) | 0.0013 (17) | 0.0016 (16) |
N2 | 0.0497 (16) | 0.0386 (16) | 0.0425 (16) | 0.0012 (12) | 0.0057 (13) | 0.0015 (12) |
C26 | 0.0463 (18) | 0.0346 (18) | 0.047 (2) | −0.0009 (14) | 0.0077 (15) | −0.0015 (15) |
C27 | 0.113 (4) | 0.051 (2) | 0.048 (2) | 0.028 (2) | −0.011 (2) | −0.0023 (19) |
C28 | 0.115 (4) | 0.050 (2) | 0.056 (3) | 0.022 (2) | −0.011 (3) | −0.017 (2) |
C29 | 0.052 (2) | 0.043 (2) | 0.050 (2) | 0.0022 (16) | 0.0087 (17) | −0.0043 (17) |
C30 | 0.082 (3) | 0.046 (2) | 0.044 (2) | 0.0075 (19) | 0.0053 (19) | 0.0052 (17) |
C31 | 0.078 (3) | 0.042 (2) | 0.041 (2) | 0.0045 (18) | 0.0054 (19) | −0.0051 (16) |
Si2 | 0.0647 (7) | 0.0433 (6) | 0.0555 (7) | 0.0092 (5) | 0.0106 (5) | 0.0002 (5) |
C32 | 0.076 (3) | 0.085 (3) | 0.088 (4) | 0.016 (2) | −0.005 (3) | −0.001 (3) |
C33 | 0.076 (3) | 0.055 (2) | 0.074 (3) | 0.012 (2) | 0.014 (2) | −0.010 (2) |
C34 | 0.123 (4) | 0.060 (3) | 0.091 (4) | 0.019 (3) | 0.035 (3) | 0.014 (3) |
C35 | 0.067 (2) | 0.046 (2) | 0.054 (2) | −0.0006 (19) | 0.015 (2) | −0.0040 (18) |
O7 | 0.091 (2) | 0.074 (2) | 0.100 (2) | −0.0246 (17) | 0.0464 (19) | −0.0035 (17) |
C36 | 0.063 (2) | 0.043 (2) | 0.055 (2) | −0.0019 (18) | 0.007 (2) | −0.0047 (18) |
O8 | 0.081 (2) | 0.080 (2) | 0.066 (2) | 0.0066 (16) | −0.0111 (17) | −0.0025 (16) |
C37 | 0.070 (3) | 0.052 (2) | 0.047 (2) | 0.0018 (19) | 0.0139 (19) | −0.0006 (18) |
O9 | 0.106 (2) | 0.0615 (19) | 0.077 (2) | 0.0133 (17) | 0.0232 (18) | −0.0179 (16) |
C38 | 0.051 (2) | 0.060 (2) | 0.080 (3) | −0.004 (2) | 0.013 (2) | −0.004 (2) |
O10 | 0.0580 (18) | 0.084 (2) | 0.129 (3) | 0.0091 (17) | 0.0044 (18) | 0.009 (2) |
C39 | 0.065 (3) | 0.063 (3) | 0.062 (3) | 0.0039 (19) | 0.019 (2) | −0.001 (2) |
O11 | 0.115 (3) | 0.105 (3) | 0.071 (2) | −0.004 (2) | 0.039 (2) | −0.0100 (19) |
C40 | 0.064 (3) | 0.067 (3) | 0.081 (3) | −0.021 (2) | 0.026 (2) | −0.007 (2) |
O12 | 0.115 (3) | 0.078 (2) | 0.145 (4) | −0.047 (2) | 0.032 (3) | −0.021 (2) |
Fe1—C17 | 1.779 (4) | Fe3—C35 | 1.786 (4) |
Fe1—C15 | 1.794 (4) | Fe3—C37 | 1.795 (4) |
Fe1—C16 | 1.802 (4) | Fe3—N2 | 1.987 (3) |
Fe1—N1 | 1.968 (3) | Fe3—C24 | 2.154 (3) |
Fe1—C4 | 2.169 (3) | Fe3—C23 | 2.271 (4) |
Fe1—C3 | 2.322 (4) | Fe3—Fe4 | 2.4570 (7) |
Fe1—Fe2 | 2.4538 (7) | Fe3—C25 | 2.635 (3) |
Fe1—C5 | 2.639 (4) | Fe4—C39 | 1.788 (5) |
Fe2—C19 | 1.770 (4) | Fe4—C40 | 1.793 (4) |
Fe2—C20 | 1.785 (5) | Fe4—C38 | 1.820 (4) |
Fe2—C18 | 1.812 (4) | Fe4—C24 | 1.938 (4) |
Fe2—C4 | 1.939 (4) | Fe4—N2 | 2.008 (3) |
Fe2—N1 | 1.991 (3) | Fe4—C36 | 2.797 (4) |
Fe2—C3 | 2.864 (4) | Fe4—C23 | 2.866 (4) |
S1—C1 | 1.717 (5) | S2—C21 | 1.715 (4) |
S1—C4 | 1.743 (3) | S2—C24 | 1.756 (3) |
C1—C2 | 1.348 (6) | C21—C22 | 1.345 (5) |
C1—H1 | 0.9300 | C21—H21 | 0.9300 |
C2—C3 | 1.429 (5) | C22—C23 | 1.430 (5) |
C2—H2 | 0.9300 | C22—H22 | 0.9300 |
C3—C4 | 1.412 (5) | C23—C24 | 1.406 (5) |
C3—C5 | 1.497 (5) | C23—C25 | 1.498 (4) |
C5—N1 | 1.486 (4) | C25—N2 | 1.495 (4) |
C5—H5A | 0.9700 | C25—H25A | 0.9700 |
C5—H5B | 0.9700 | C25—H25B | 0.9700 |
N1—C6 | 1.447 (4) | N2—C26 | 1.446 (4) |
C6—C11 | 1.363 (5) | C26—C31 | 1.368 (5) |
C6—C7 | 1.393 (5) | C26—C27 | 1.369 (5) |
C7—C8 | 1.385 (5) | C27—C28 | 1.402 (5) |
C7—H7 | 0.9300 | C27—H27 | 0.9300 |
C8—C9 | 1.386 (5) | C28—C29 | 1.375 (5) |
C8—H8 | 0.9300 | C28—H28 | 0.9300 |
C9—C10 | 1.370 (5) | C29—C30 | 1.374 (5) |
C9—Si1 | 1.875 (4) | C29—Si2 | 1.878 (3) |
C10—C11 | 1.386 (5) | C30—C31 | 1.397 (5) |
C10—H10 | 0.9300 | C30—H30 | 0.9300 |
C11—H11 | 0.9300 | C31—H31 | 0.9300 |
Si1—C14 | 1.849 (4) | Si2—C33 | 1.850 (4) |
Si1—C13 | 1.852 (5) | Si2—C32 | 1.856 (4) |
Si1—C12 | 1.858 (4) | Si2—C34 | 1.860 (5) |
C12—H12A | 0.9600 | C32—H32A | 0.9600 |
C12—H12B | 0.9600 | C32—H32B | 0.9600 |
C12—H12C | 0.9600 | C32—H32C | 0.9600 |
C13—H13A | 0.9600 | C33—H33A | 0.9600 |
C13—H13B | 0.9600 | C33—H33B | 0.9600 |
C13—H13C | 0.9600 | C33—H33C | 0.9600 |
C14—H14A | 0.9600 | C34—H34A | 0.9600 |
C14—H14B | 0.9600 | C34—H34B | 0.9600 |
C14—H14C | 0.9600 | C34—H34C | 0.9600 |
C15—O1 | 1.132 (5) | C35—O7 | 1.141 (4) |
C16—O2 | 1.131 (5) | C36—O8 | 1.159 (4) |
C17—O3 | 1.141 (5) | C37—O9 | 1.140 (4) |
C18—O4 | 1.138 (5) | C38—O10 | 1.138 (5) |
C19—O5 | 1.151 (5) | C39—O11 | 1.145 (5) |
C20—O6 | 1.142 (5) | C40—O12 | 1.123 (5) |
Fe3—C36 | 1.769 (4) | ||
C17—Fe1—C15 | 101.74 (19) | C37—Fe3—N2 | 162.56 (14) |
C17—Fe1—C16 | 91.60 (18) | C36—Fe3—C24 | 121.83 (16) |
C15—Fe1—C16 | 92.62 (18) | C35—Fe3—C24 | 133.91 (16) |
C17—Fe1—N1 | 96.87 (15) | C37—Fe3—C24 | 89.44 (15) |
C15—Fe1—N1 | 100.72 (15) | N2—Fe3—C24 | 73.42 (12) |
C16—Fe1—N1 | 162.37 (15) | C36—Fe3—C23 | 155.55 (16) |
C17—Fe1—C4 | 128.30 (16) | C35—Fe3—C23 | 97.79 (16) |
C15—Fe1—C4 | 129.85 (18) | C37—Fe3—C23 | 99.54 (15) |
C16—Fe1—C4 | 89.45 (15) | N2—Fe3—C23 | 64.82 (11) |
N1—Fe1—C4 | 73.16 (12) | C24—Fe3—C23 | 36.92 (13) |
C17—Fe1—C3 | 156.76 (15) | C36—Fe3—Fe4 | 81.11 (13) |
C15—Fe1—C3 | 95.16 (17) | C35—Fe3—Fe4 | 149.70 (12) |
C16—Fe1—C3 | 103.55 (16) | C37—Fe3—Fe4 | 117.99 (13) |
N1—Fe1—C3 | 64.07 (12) | N2—Fe3—Fe4 | 52.42 (8) |
C4—Fe1—C3 | 36.45 (13) | C24—Fe3—Fe4 | 49.16 (9) |
C17—Fe1—Fe2 | 84.20 (12) | C23—Fe3—Fe4 | 74.51 (9) |
C15—Fe1—Fe2 | 152.82 (13) | C36—Fe3—C25 | 135.60 (14) |
C16—Fe1—Fe2 | 113.88 (13) | C35—Fe3—C25 | 86.89 (15) |
N1—Fe1—Fe2 | 52.11 (8) | C37—Fe3—C25 | 132.83 (14) |
C4—Fe1—Fe2 | 49.11 (9) | N2—Fe3—C25 | 34.24 (10) |
C3—Fe1—Fe2 | 73.64 (9) | C24—Fe3—C25 | 59.99 (12) |
C17—Fe1—C5 | 130.21 (15) | C23—Fe3—C25 | 34.56 (11) |
C15—Fe1—C5 | 87.04 (16) | Fe4—Fe3—C25 | 70.06 (8) |
C16—Fe1—C5 | 137.37 (16) | C39—Fe4—C40 | 97.9 (2) |
N1—Fe1—C5 | 33.83 (11) | C39—Fe4—C38 | 95.94 (19) |
C4—Fe1—C5 | 59.94 (13) | C40—Fe4—C38 | 91.70 (19) |
C3—Fe1—C5 | 34.39 (11) | C39—Fe4—C24 | 97.05 (17) |
Fe2—Fe1—C5 | 69.63 (8) | C40—Fe4—C24 | 91.41 (18) |
C19—Fe2—C20 | 96.62 (19) | C38—Fe4—C24 | 166.10 (17) |
C19—Fe2—C18 | 92.49 (19) | C39—Fe4—N2 | 103.50 (16) |
C20—Fe2—C18 | 97.92 (18) | C40—Fe4—N2 | 157.05 (16) |
C19—Fe2—C4 | 92.63 (18) | C38—Fe4—N2 | 94.33 (14) |
C20—Fe2—C4 | 94.32 (16) | C24—Fe4—N2 | 77.85 (13) |
C18—Fe2—C4 | 166.10 (16) | C39—Fe4—Fe3 | 144.97 (14) |
C19—Fe2—N1 | 156.80 (16) | C40—Fe4—Fe3 | 105.47 (14) |
C20—Fe2—N1 | 105.10 (16) | C38—Fe4—Fe3 | 108.89 (13) |
C18—Fe2—N1 | 92.50 (15) | C24—Fe4—Fe3 | 57.25 (10) |
C4—Fe2—N1 | 77.90 (13) | N2—Fe4—Fe3 | 51.68 (8) |
C19—Fe2—Fe1 | 105.77 (14) | C39—Fe4—C36 | 169.94 (15) |
C20—Fe2—Fe1 | 144.23 (14) | C40—Fe4—C36 | 87.75 (16) |
C18—Fe2—Fe1 | 108.38 (13) | C38—Fe4—C36 | 75.46 (16) |
C4—Fe2—Fe1 | 57.76 (10) | C24—Fe4—C36 | 91.13 (13) |
N1—Fe2—Fe1 | 51.28 (8) | N2—Fe4—C36 | 72.45 (11) |
C19—Fe2—C3 | 118.60 (16) | Fe3—Fe4—C36 | 38.68 (8) |
C20—Fe2—C3 | 93.77 (15) | C39—Fe4—C23 | 96.35 (15) |
C18—Fe2—C3 | 145.22 (15) | C40—Fe4—C23 | 117.01 (16) |
C4—Fe2—C3 | 26.16 (13) | C38—Fe4—C23 | 146.70 (14) |
N1—Fe2—C3 | 52.78 (10) | C24—Fe4—C23 | 25.88 (12) |
Fe1—Fe2—C3 | 51.07 (8) | N2—Fe4—C23 | 52.68 (10) |
C1—S1—C4 | 92.5 (2) | Fe3—Fe4—C23 | 49.79 (7) |
C2—C1—S1 | 113.5 (3) | C36—Fe4—C23 | 88.45 (11) |
C2—C1—H1 | 123.2 | C21—S2—C24 | 92.49 (18) |
S1—C1—H1 | 123.2 | C22—C21—S2 | 113.4 (3) |
C1—C2—C3 | 111.4 (4) | C22—C21—H21 | 123.3 |
C1—C2—H2 | 124.3 | S2—C21—H21 | 123.3 |
C3—C2—H2 | 124.3 | C21—C22—C23 | 111.6 (4) |
C4—C3—C2 | 114.2 (3) | C21—C22—H22 | 124.2 |
C4—C3—C5 | 113.6 (3) | C23—C22—H22 | 124.2 |
C2—C3—C5 | 130.2 (4) | C24—C23—C22 | 114.4 (3) |
C4—C3—Fe1 | 65.9 (2) | C24—C23—C25 | 113.6 (3) |
C2—C3—Fe1 | 127.7 (3) | C22—C23—C25 | 129.6 (3) |
C5—C3—Fe1 | 84.5 (2) | C24—C23—Fe3 | 67.0 (2) |
C4—C3—Fe2 | 37.24 (17) | C22—C23—Fe3 | 126.5 (3) |
C2—C3—Fe2 | 151.1 (3) | C25—C23—Fe3 | 86.1 (2) |
C5—C3—Fe2 | 76.72 (19) | C24—C23—Fe4 | 37.00 (17) |
Fe1—C3—Fe2 | 55.29 (8) | C22—C23—Fe4 | 151.3 (3) |
C3—C4—S1 | 108.4 (3) | C25—C23—Fe4 | 77.26 (19) |
C3—C4—Fe2 | 116.6 (3) | Fe3—C23—Fe4 | 55.71 (8) |
S1—C4—Fe2 | 134.6 (2) | C23—C24—S2 | 108.0 (3) |
C3—C4—Fe1 | 77.7 (2) | C23—C24—Fe4 | 117.1 (3) |
S1—C4—Fe1 | 124.32 (18) | S2—C24—Fe4 | 134.6 (2) |
Fe2—C4—Fe1 | 73.13 (12) | C23—C24—Fe3 | 76.1 (2) |
N1—C5—C3 | 100.6 (3) | S2—C24—Fe3 | 124.60 (18) |
N1—C5—Fe1 | 47.50 (15) | Fe4—C24—Fe3 | 73.59 (12) |
C3—C5—Fe1 | 61.16 (19) | N2—C25—C23 | 100.1 (3) |
N1—C5—H5A | 111.7 | N2—C25—Fe3 | 48.42 (14) |
C3—C5—H5A | 111.7 | C23—C25—Fe3 | 59.30 (18) |
Fe1—C5—H5A | 148.5 | N2—C25—H25A | 111.7 |
N1—C5—H5B | 111.7 | C23—C25—H25A | 111.7 |
C3—C5—H5B | 111.7 | Fe3—C25—H25A | 102.0 |
Fe1—C5—H5B | 101.2 | N2—C25—H25B | 111.7 |
H5A—C5—H5B | 109.4 | C23—C25—H25B | 111.7 |
C6—N1—C5 | 110.5 (3) | Fe3—C25—H25B | 148.0 |
C6—N1—Fe1 | 130.3 (2) | H25A—C25—H25B | 109.5 |
C5—N1—Fe1 | 98.7 (2) | C26—N2—C25 | 112.6 (2) |
C6—N1—Fe2 | 122.9 (2) | C26—N2—Fe3 | 132.1 (2) |
C5—N1—Fe2 | 112.9 (2) | C25—N2—Fe3 | 97.34 (19) |
Fe1—N1—Fe2 | 76.61 (10) | C26—N2—Fe4 | 120.6 (2) |
C11—C6—C7 | 117.6 (3) | C25—N2—Fe4 | 112.5 (2) |
C11—C6—N1 | 123.8 (3) | Fe3—N2—Fe4 | 75.90 (9) |
C7—C6—N1 | 118.6 (3) | C31—C26—C27 | 118.1 (3) |
C8—C7—C6 | 119.9 (4) | C31—C26—N2 | 122.2 (3) |
C8—C7—H7 | 120.0 | C27—C26—N2 | 119.7 (3) |
C6—C7—H7 | 120.0 | C26—C27—C28 | 120.6 (3) |
C9—C8—C7 | 123.1 (4) | C26—C27—H27 | 119.7 |
C9—C8—H8 | 118.4 | C28—C27—H27 | 119.7 |
C7—C8—H8 | 118.4 | C29—C28—C27 | 122.6 (4) |
C10—C9—C8 | 115.1 (4) | C29—C28—H28 | 118.7 |
C10—C9—Si1 | 124.4 (3) | C27—C28—H28 | 118.7 |
C8—C9—Si1 | 120.5 (3) | C28—C29—C30 | 115.1 (3) |
C9—C10—C11 | 123.0 (4) | C28—C29—Si2 | 121.3 (3) |
C9—C10—H10 | 118.5 | C30—C29—Si2 | 123.5 (3) |
C11—C10—H10 | 118.5 | C29—C30—C31 | 123.4 (3) |
C6—C11—C10 | 121.2 (4) | C29—C30—H30 | 118.3 |
C6—C11—H11 | 119.4 | C31—C30—H30 | 118.3 |
C10—C11—H11 | 119.4 | C26—C31—C30 | 120.2 (3) |
C14—Si1—C13 | 108.9 (2) | C26—C31—H31 | 119.9 |
C14—Si1—C12 | 110.0 (2) | C30—C31—H31 | 119.9 |
C13—Si1—C12 | 109.9 (2) | C33—Si2—C32 | 109.5 (2) |
C14—Si1—C9 | 109.68 (19) | C33—Si2—C34 | 110.4 (2) |
C13—Si1—C9 | 109.4 (2) | C32—Si2—C34 | 109.8 (2) |
C12—Si1—C9 | 109.00 (19) | C33—Si2—C29 | 109.15 (18) |
Si1—C12—H12A | 109.5 | C32—Si2—C29 | 108.57 (19) |
Si1—C12—H12B | 109.5 | C34—Si2—C29 | 109.48 (19) |
H12A—C12—H12B | 109.5 | Si2—C32—H32A | 109.5 |
Si1—C12—H12C | 109.5 | Si2—C32—H32B | 109.5 |
H12A—C12—H12C | 109.5 | H32A—C32—H32B | 109.5 |
H12B—C12—H12C | 109.5 | Si2—C32—H32C | 109.5 |
Si1—C13—H13A | 109.5 | H32A—C32—H32C | 109.5 |
Si1—C13—H13B | 109.5 | H32B—C32—H32C | 109.5 |
H13A—C13—H13B | 109.5 | Si2—C33—H33A | 109.5 |
Si1—C13—H13C | 109.5 | Si2—C33—H33B | 109.5 |
H13A—C13—H13C | 109.5 | H33A—C33—H33B | 109.5 |
H13B—C13—H13C | 109.5 | Si2—C33—H33C | 109.5 |
Si1—C14—H14A | 109.5 | H33A—C33—H33C | 109.5 |
Si1—C14—H14B | 109.5 | H33B—C33—H33C | 109.5 |
H14A—C14—H14B | 109.5 | Si2—C34—H34A | 109.5 |
Si1—C14—H14C | 109.5 | Si2—C34—H34B | 109.5 |
H14A—C14—H14C | 109.5 | H34A—C34—H34B | 109.5 |
H14B—C14—H14C | 109.5 | Si2—C34—H34C | 109.5 |
O1—C15—Fe1 | 175.9 (4) | H34A—C34—H34C | 109.5 |
O2—C16—Fe1 | 178.3 (4) | H34B—C34—H34C | 109.5 |
O3—C17—Fe1 | 176.5 (4) | O7—C35—Fe3 | 178.3 (4) |
O4—C18—Fe2 | 178.7 (4) | O8—C36—Fe3 | 173.3 (4) |
O5—C19—Fe2 | 178.8 (4) | O8—C36—Fe4 | 125.5 (3) |
O6—C20—Fe2 | 176.9 (4) | Fe3—C36—Fe4 | 60.22 (12) |
C36—Fe3—C35 | 104.23 (18) | O9—C37—Fe3 | 178.1 (4) |
C36—Fe3—C37 | 90.27 (17) | O10—C38—Fe4 | 177.0 (4) |
C35—Fe3—C37 | 92.03 (17) | O11—C39—Fe4 | 177.5 (4) |
C36—Fe3—N2 | 101.36 (14) | O12—C40—Fe4 | 178.3 (4) |
C35—Fe3—N2 | 97.56 (14) |
D—H···A | H···A | D···A | D—H···A |
C12—H12A···O1i | 2.80 | 3.668 (5) | 151 |
C33—H33B···O4ii | 2.78 | 3.376 (6) | 121 |
C33—H33A···O7iii | 2.74 | 3.567 (6) | 145 |
C25—H25B···O9iv | 2.77 | 3.458 (5) | 129 |
C34—H34C···O11v | 2.77 | 3.521 (6) | 136 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) x, −y−1/2, z−1/2; (iii) −x, y−1/2, −z−1/2; (iv) x, −y+1/2, z−1/2; (v) x, −y−1/2, z+1/2. |