Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229621008500/yo3080sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229621008500/yo30802sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229621008500/yo30803sup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229621008500/yo30804sup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229621008500/yo30805sup5.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229621008500/yo3080sup6.pdf |
CCDC references: 2063936; 2063937; 2063938; 2063939
Data collection: SMART (Bruker, 2002) for (2), (3), (4); APEX2 (Bruker, 2007) for (5). Cell refinement: SAINT (Bruker, 2002) for (2), (3), (4); SAINT (Bruker, 2007) for (5). Data reduction: SAINT (Bruker, 2002) for (2), (3), (4); SAINT (Bruker, 2007) for (5). Program(s) used to solve structure: SHELXS1997 (Sheldrick, 2008) for (2), (3), (4); SHELXT (Sheldrick, 2015a) for (5). Program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015b) for (2), (4), (5); SHELXXL2018 (Sheldrick, 2015b) for (3). For all structures, molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).
[Fe(C21H38BS3)(C19H15O)] | Z = 2 |
Mr = 712.66 | F(000) = 760 |
Triclinic, P1 | Dx = 1.212 Mg m−3 |
a = 10.6835 (15) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.8042 (18) Å | Cell parameters from 989 reflections |
c = 15.795 (2) Å | θ = 1.7–25.2° |
α = 77.614 (3)° | µ = 0.58 mm−1 |
β = 75.849 (3)° | T = 200 K |
γ = 70.332 (3)° | Block, colourless |
V = 1952.1 (5) Å3 | 0.34 × 0.28 × 0.20 mm |
Bruker APEX diffractometer | 9591 independent reflections |
Radiation source: fine focus sealed tube | 6143 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
Detector resolution: 8.33 pixels mm-1 | θmax = 28.3°, θmin = 1.7° |
ω scans | h = −14→14 |
Absorption correction: multi-scan SADABS (Bruker, 2002) | k = −17→17 |
Tmin = 0.830, Tmax = 0.893 | l = −21→21 |
19244 measured reflections |
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)] = 0.055 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.130 | H-atom parameters constrained |
S = 0.98 | w = 1/[σ2(Fo2) + (0.0461P)2] where P = (Fo2 + 2Fc2)/3 |
9591 reflections | (Δ/σ)max < 0.001 |
424 parameters | Δρmax = 0.53 e Å−3 |
0 restraints | Δρmin = −0.39 e Å−3 |
Experimental. Data collection is performed with four batch runs at φ = 0.00 \ (600 frames), at φ = 90.00 \ (600 frames), at φ = 180 \ (600 frames) and at φ = 270 \ (600 frames). Frame width = 0.30 \& in ω. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 | ||
Fe1 | 0.19751 (4) | 0.24770 (3) | 0.28435 (2) | 0.02585 (12) | |
B1 | 0.2720 (3) | 0.3028 (3) | 0.4682 (2) | 0.0270 (7) | |
O1 | 0.10047 (19) | 0.24057 (16) | 0.20615 (12) | 0.0292 (4) | |
S1 | 0.09664 (7) | 0.18654 (6) | 0.43517 (4) | 0.02835 (17) | |
S2 | 0.15430 (7) | 0.43591 (6) | 0.31471 (4) | 0.02661 (17) | |
S3 | 0.42450 (7) | 0.18261 (6) | 0.31420 (4) | 0.02664 (17) | |
C1 | 0.2472 (3) | 0.3238 (3) | 0.6387 (2) | 0.0407 (8) | |
H1 | 0.165936 | 0.303617 | 0.651972 | 0.049* | |
C2 | 0.2903 (4) | 0.3465 (3) | 0.7071 (2) | 0.0486 (9) | |
H2 | 0.239346 | 0.340754 | 0.765350 | 0.058* | |
C3 | 0.4064 (4) | 0.3771 (3) | 0.6906 (2) | 0.0456 (9) | |
H3 | 0.436533 | 0.392465 | 0.737172 | 0.055* | |
C4 | 0.4789 (3) | 0.3854 (3) | 0.6048 (2) | 0.0413 (8) | |
H4 | 0.558713 | 0.407530 | 0.591939 | 0.050* | |
C5 | 0.4347 (3) | 0.3613 (2) | 0.53846 (19) | 0.0335 (7) | |
H5 | 0.486668 | 0.366671 | 0.480455 | 0.040* | |
C6 | 0.3171 (3) | 0.3292 (2) | 0.55163 (18) | 0.0281 (6) | |
C7 | 0.1273 (3) | 0.2722 (3) | 0.50169 (18) | 0.0335 (7) | |
H7A | 0.052309 | 0.343271 | 0.503004 | 0.040* | |
H7B | 0.124606 | 0.232573 | 0.562951 | 0.040* | |
C8 | 0.2560 (3) | 0.4199 (2) | 0.39606 (18) | 0.0318 (7) | |
H8A | 0.347464 | 0.422587 | 0.364662 | 0.038* | |
H8B | 0.215329 | 0.484687 | 0.429070 | 0.038* | |
C9 | 0.3981 (3) | 0.1968 (2) | 0.43061 (17) | 0.0309 (7) | |
H9A | 0.384034 | 0.126676 | 0.466359 | 0.037* | |
H9B | 0.482678 | 0.202750 | 0.441510 | 0.037* | |
C10 | −0.0909 (3) | 0.2228 (3) | 0.44938 (19) | 0.0322 (7) | |
C11 | −0.1472 (3) | 0.2017 (3) | 0.5481 (2) | 0.0464 (9) | |
H11A | −0.128992 | 0.252795 | 0.578412 | 0.070* | |
H11B | −0.103602 | 0.124052 | 0.571788 | 0.070* | |
H11C | −0.245055 | 0.214903 | 0.557283 | 0.070* | |
C12 | −0.1514 (3) | 0.3436 (3) | 0.4098 (2) | 0.0423 (8) | |
H12A | −0.114655 | 0.353604 | 0.346336 | 0.063* | |
H12B | −0.128536 | 0.393806 | 0.438301 | 0.063* | |
H12C | −0.249986 | 0.361221 | 0.419084 | 0.063* | |
C13 | −0.1147 (3) | 0.1421 (3) | 0.4017 (2) | 0.0393 (8) | |
H13A | −0.212203 | 0.156671 | 0.406809 | 0.059* | |
H13B | −0.074802 | 0.064879 | 0.428195 | 0.059* | |
H13C | −0.072535 | 0.152613 | 0.339245 | 0.059* | |
C14 | 0.2087 (3) | 0.5349 (2) | 0.22052 (18) | 0.0292 (6) | |
C15 | 0.1792 (4) | 0.6465 (2) | 0.2529 (2) | 0.0432 (8) | |
H15A | 0.235985 | 0.636560 | 0.295994 | 0.065* | |
H15B | 0.083650 | 0.672131 | 0.280667 | 0.065* | |
H15C | 0.199166 | 0.702270 | 0.202740 | 0.065* | |
C16 | 0.1198 (3) | 0.5484 (3) | 0.15408 (19) | 0.0386 (8) | |
H16A | 0.140559 | 0.602373 | 0.102682 | 0.058* | |
H16B | 0.024345 | 0.575637 | 0.181683 | 0.058* | |
H16C | 0.137487 | 0.475828 | 0.135246 | 0.058* | |
C17 | 0.3583 (3) | 0.4902 (3) | 0.1811 (2) | 0.0413 (8) | |
H17A | 0.376216 | 0.417071 | 0.163168 | 0.062* | |
H17B | 0.412612 | 0.482015 | 0.225324 | 0.062* | |
H17C | 0.382354 | 0.542697 | 0.129581 | 0.062* | |
C18 | 0.5197 (3) | 0.0323 (2) | 0.30736 (18) | 0.0277 (6) | |
C19 | 0.4387 (3) | −0.0435 (2) | 0.36444 (19) | 0.0359 (7) | |
H19A | 0.488941 | −0.121753 | 0.357529 | 0.054* | |
H19B | 0.351316 | −0.023634 | 0.346194 | 0.054* | |
H19C | 0.423752 | −0.033913 | 0.426414 | 0.054* | |
C20 | 0.6548 (3) | 0.0082 (3) | 0.3351 (2) | 0.0394 (8) | |
H20A | 0.638739 | 0.022415 | 0.395930 | 0.059* | |
H20B | 0.705026 | 0.057082 | 0.295839 | 0.059* | |
H20C | 0.707515 | −0.070322 | 0.331209 | 0.059* | |
C21 | 0.5441 (3) | 0.0194 (3) | 0.21037 (18) | 0.0359 (7) | |
H21A | 0.596201 | −0.058229 | 0.202403 | 0.054* | |
H21B | 0.594750 | 0.069874 | 0.174485 | 0.054* | |
H21C | 0.456997 | 0.038239 | 0.191909 | 0.054* | |
C22 | 0.1228 (3) | 0.2040 (2) | 0.12385 (17) | 0.0249 (6) | |
C23 | 0.1989 (3) | 0.0073 (2) | 0.20533 (18) | 0.0298 (7) | |
H23 | 0.135686 | 0.033741 | 0.255704 | 0.036* | |
C24 | 0.2761 (3) | −0.1043 (3) | 0.2107 (2) | 0.0371 (7) | |
H24 | 0.265581 | −0.153506 | 0.264501 | 0.044* | |
C25 | 0.3681 (3) | −0.1443 (2) | 0.1383 (2) | 0.0351 (7) | |
H25 | 0.421842 | −0.220589 | 0.142312 | 0.042* | |
C26 | 0.3818 (3) | −0.0730 (2) | 0.06024 (19) | 0.0322 (7) | |
H26 | 0.444722 | −0.100335 | 0.010051 | 0.039* | |
C27 | 0.3039 (3) | 0.0385 (2) | 0.05472 (18) | 0.0281 (6) | |
H27 | 0.313195 | 0.086610 | 0.000197 | 0.034* | |
C28 | 0.2122 (3) | 0.0816 (2) | 0.12741 (17) | 0.0250 (6) | |
C29 | 0.3209 (3) | 0.2810 (2) | 0.05584 (18) | 0.0291 (6) | |
H29 | 0.368878 | 0.227908 | 0.097811 | 0.035* | |
C30 | 0.3813 (3) | 0.3551 (2) | −0.00160 (19) | 0.0337 (7) | |
H30 | 0.469929 | 0.352911 | 0.001260 | 0.040* | |
C31 | 0.3134 (3) | 0.4325 (3) | −0.06335 (19) | 0.0355 (7) | |
H31 | 0.355039 | 0.483633 | −0.103067 | 0.043* | |
C32 | 0.1857 (3) | 0.4350 (2) | −0.06678 (19) | 0.0343 (7) | |
H32 | 0.138892 | 0.488005 | −0.109345 | 0.041* | |
C33 | 0.1233 (3) | 0.3609 (2) | −0.00876 (18) | 0.0300 (7) | |
H33 | 0.034394 | 0.364146 | −0.011827 | 0.036* | |
C34 | 0.1902 (3) | 0.2823 (2) | 0.05359 (17) | 0.0238 (6) | |
C35 | −0.0181 (3) | 0.1609 (3) | 0.0345 (2) | 0.0433 (8) | |
H35 | 0.064091 | 0.124473 | −0.001183 | 0.052* | |
C36 | −0.1396 (4) | 0.1652 (3) | 0.0158 (3) | 0.0542 (10) | |
H36 | −0.140658 | 0.132988 | −0.032829 | 0.065* | |
C37 | −0.2582 (4) | 0.2162 (3) | 0.0676 (3) | 0.0582 (11) | |
H37 | −0.342015 | 0.218968 | 0.055211 | 0.070* | |
C38 | −0.2570 (3) | 0.2636 (3) | 0.1380 (3) | 0.0527 (10) | |
H38 | −0.339743 | 0.298393 | 0.174157 | 0.063* | |
C39 | −0.1334 (3) | 0.2605 (3) | 0.1561 (2) | 0.0390 (8) | |
H39 | −0.132511 | 0.294135 | 0.203939 | 0.047* | |
C40 | −0.0131 (3) | 0.2086 (2) | 0.10442 (19) | 0.0299 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0259 (2) | 0.0278 (2) | 0.0252 (2) | −0.00956 (18) | −0.00482 (17) | −0.00413 (18) |
B1 | 0.0271 (18) | 0.0312 (18) | 0.0246 (16) | −0.0107 (15) | −0.0056 (14) | −0.0039 (14) |
O1 | 0.0276 (11) | 0.0359 (12) | 0.0259 (10) | −0.0105 (9) | −0.0033 (8) | −0.0091 (9) |
S1 | 0.0275 (4) | 0.0313 (4) | 0.0267 (4) | −0.0116 (3) | −0.0022 (3) | −0.0041 (3) |
S2 | 0.0285 (4) | 0.0253 (4) | 0.0272 (4) | −0.0098 (3) | −0.0063 (3) | −0.0024 (3) |
S3 | 0.0258 (4) | 0.0258 (4) | 0.0273 (4) | −0.0065 (3) | −0.0055 (3) | −0.0032 (3) |
C1 | 0.0390 (19) | 0.048 (2) | 0.0364 (18) | −0.0121 (16) | −0.0050 (15) | −0.0135 (16) |
C2 | 0.052 (2) | 0.067 (2) | 0.0298 (17) | −0.017 (2) | −0.0056 (16) | −0.0163 (17) |
C3 | 0.053 (2) | 0.050 (2) | 0.0409 (19) | −0.0094 (18) | −0.0216 (17) | −0.0160 (17) |
C4 | 0.043 (2) | 0.0374 (19) | 0.051 (2) | −0.0147 (16) | −0.0186 (16) | −0.0066 (16) |
C5 | 0.0381 (18) | 0.0353 (17) | 0.0297 (16) | −0.0129 (15) | −0.0081 (13) | −0.0049 (14) |
C6 | 0.0321 (16) | 0.0237 (15) | 0.0269 (15) | −0.0046 (13) | −0.0087 (13) | −0.0025 (12) |
C7 | 0.0405 (18) | 0.0393 (18) | 0.0257 (15) | −0.0157 (15) | −0.0067 (13) | −0.0081 (13) |
C8 | 0.0378 (18) | 0.0329 (17) | 0.0295 (15) | −0.0127 (14) | −0.0109 (13) | −0.0059 (13) |
C9 | 0.0355 (17) | 0.0320 (17) | 0.0269 (15) | −0.0069 (14) | −0.0128 (13) | −0.0051 (13) |
C10 | 0.0259 (16) | 0.0367 (17) | 0.0341 (16) | −0.0139 (14) | 0.0021 (13) | −0.0070 (14) |
C11 | 0.0367 (19) | 0.062 (2) | 0.0392 (19) | −0.0190 (18) | 0.0078 (15) | −0.0136 (17) |
C12 | 0.0308 (18) | 0.0396 (19) | 0.054 (2) | −0.0088 (15) | −0.0053 (15) | −0.0077 (17) |
C13 | 0.0352 (18) | 0.044 (2) | 0.0447 (19) | −0.0196 (16) | −0.0034 (15) | −0.0111 (16) |
C14 | 0.0351 (17) | 0.0271 (16) | 0.0276 (15) | −0.0133 (14) | −0.0080 (13) | 0.0006 (12) |
C15 | 0.061 (2) | 0.0301 (18) | 0.047 (2) | −0.0232 (17) | −0.0144 (17) | −0.0034 (15) |
C16 | 0.045 (2) | 0.0373 (18) | 0.0346 (17) | −0.0129 (16) | −0.0163 (15) | 0.0026 (14) |
C17 | 0.0375 (19) | 0.056 (2) | 0.0337 (17) | −0.0221 (17) | −0.0056 (14) | −0.0022 (16) |
C18 | 0.0282 (16) | 0.0241 (15) | 0.0299 (15) | −0.0043 (13) | −0.0071 (12) | −0.0058 (12) |
C19 | 0.048 (2) | 0.0259 (16) | 0.0350 (17) | −0.0140 (15) | −0.0097 (15) | 0.0010 (13) |
C20 | 0.0328 (18) | 0.0370 (18) | 0.0488 (19) | −0.0039 (15) | −0.0139 (15) | −0.0106 (15) |
C21 | 0.0347 (18) | 0.0374 (18) | 0.0345 (17) | −0.0085 (15) | −0.0012 (14) | −0.0126 (14) |
C22 | 0.0231 (15) | 0.0269 (15) | 0.0252 (14) | −0.0067 (12) | −0.0062 (12) | −0.0045 (12) |
C23 | 0.0315 (17) | 0.0315 (17) | 0.0278 (15) | −0.0140 (14) | 0.0010 (13) | −0.0076 (13) |
C24 | 0.048 (2) | 0.0328 (18) | 0.0327 (17) | −0.0197 (16) | −0.0055 (15) | 0.0000 (14) |
C25 | 0.0351 (18) | 0.0246 (16) | 0.0474 (19) | −0.0081 (14) | −0.0090 (15) | −0.0088 (15) |
C26 | 0.0293 (17) | 0.0342 (17) | 0.0347 (16) | −0.0114 (14) | −0.0006 (13) | −0.0111 (14) |
C27 | 0.0320 (16) | 0.0284 (16) | 0.0272 (15) | −0.0127 (13) | −0.0063 (12) | −0.0039 (13) |
C28 | 0.0232 (15) | 0.0282 (15) | 0.0275 (14) | −0.0094 (12) | −0.0087 (12) | −0.0052 (12) |
C29 | 0.0267 (16) | 0.0266 (16) | 0.0323 (16) | −0.0064 (13) | −0.0065 (13) | −0.0024 (13) |
C30 | 0.0261 (16) | 0.0354 (18) | 0.0389 (17) | −0.0099 (14) | −0.0012 (14) | −0.0082 (15) |
C31 | 0.0395 (19) | 0.0339 (18) | 0.0309 (16) | −0.0143 (15) | 0.0007 (14) | −0.0032 (14) |
C32 | 0.0379 (19) | 0.0327 (17) | 0.0299 (16) | −0.0079 (15) | −0.0109 (14) | 0.0011 (13) |
C33 | 0.0266 (16) | 0.0305 (16) | 0.0336 (16) | −0.0062 (13) | −0.0089 (13) | −0.0064 (13) |
C34 | 0.0258 (15) | 0.0239 (14) | 0.0225 (14) | −0.0077 (12) | −0.0035 (12) | −0.0056 (12) |
C35 | 0.041 (2) | 0.049 (2) | 0.051 (2) | −0.0191 (17) | −0.0223 (16) | −0.0053 (17) |
C36 | 0.054 (2) | 0.048 (2) | 0.073 (3) | −0.021 (2) | −0.035 (2) | 0.000 (2) |
C37 | 0.047 (2) | 0.049 (2) | 0.089 (3) | −0.026 (2) | −0.042 (2) | 0.022 (2) |
C38 | 0.0276 (19) | 0.051 (2) | 0.070 (3) | −0.0128 (17) | −0.0079 (18) | 0.013 (2) |
C39 | 0.0298 (18) | 0.0363 (18) | 0.0462 (19) | −0.0101 (15) | −0.0091 (15) | 0.0066 (15) |
C40 | 0.0271 (16) | 0.0298 (16) | 0.0346 (16) | −0.0143 (13) | −0.0088 (13) | 0.0043 (13) |
Fe1—O1 | 1.8295 (18) | C16—H16C | 0.9800 |
Fe1—S1 | 2.4417 (8) | C17—H17A | 0.9800 |
Fe1—S2 | 2.4268 (9) | C17—H17B | 0.9800 |
Fe1—S3 | 2.4141 (9) | C17—H17C | 0.9800 |
B1—C6 | 1.642 (4) | C18—C19 | 1.520 (4) |
B1—C7 | 1.655 (4) | C18—C20 | 1.523 (4) |
B1—C8 | 1.663 (4) | C18—C21 | 1.525 (4) |
B1—C9 | 1.653 (4) | C19—H19A | 0.9800 |
O1—C22 | 1.415 (3) | C19—H19B | 0.9800 |
S1—C7 | 1.822 (3) | C19—H19C | 0.9800 |
S1—C10 | 1.865 (3) | C20—H20A | 0.9800 |
S2—C8 | 1.815 (3) | C20—H20B | 0.9800 |
S2—C14 | 1.850 (3) | C20—H20C | 0.9800 |
S3—C9 | 1.830 (3) | C21—H21A | 0.9800 |
S3—C18 | 1.863 (3) | C21—H21B | 0.9800 |
C1—H1 | 0.9500 | C21—H21C | 0.9800 |
C1—C2 | 1.389 (4) | C22—C28 | 1.534 (4) |
C1—C6 | 1.396 (4) | C22—C34 | 1.541 (4) |
C2—H2 | 0.9500 | C22—C40 | 1.536 (4) |
C2—C3 | 1.373 (5) | C23—H23 | 0.9500 |
C3—H3 | 0.9500 | C23—C24 | 1.385 (4) |
C3—C4 | 1.389 (4) | C23—C28 | 1.394 (4) |
C4—H4 | 0.9500 | C24—H24 | 0.9500 |
C4—C5 | 1.377 (4) | C24—C25 | 1.377 (4) |
C5—H5 | 0.9500 | C25—H25 | 0.9500 |
C5—C6 | 1.404 (4) | C25—C26 | 1.376 (4) |
C7—H7A | 0.9900 | C26—H26 | 0.9500 |
C7—H7B | 0.9900 | C26—C27 | 1.387 (4) |
C8—H8A | 0.9900 | C27—H27 | 0.9500 |
C8—H8B | 0.9900 | C27—C28 | 1.393 (4) |
C9—H9A | 0.9900 | C29—H29 | 0.9500 |
C9—H9B | 0.9900 | C29—C30 | 1.377 (4) |
C10—C11 | 1.528 (4) | C29—C34 | 1.399 (4) |
C10—C12 | 1.521 (4) | C30—H30 | 0.9500 |
C10—C13 | 1.518 (4) | C30—C31 | 1.381 (4) |
C11—H11A | 0.9800 | C31—H31 | 0.9500 |
C11—H11B | 0.9800 | C31—C32 | 1.369 (4) |
C11—H11C | 0.9800 | C32—H32 | 0.9500 |
C12—H12A | 0.9800 | C32—C33 | 1.392 (4) |
C12—H12B | 0.9800 | C33—H33 | 0.9500 |
C12—H12C | 0.9800 | C33—C34 | 1.388 (4) |
C13—H13A | 0.9800 | C35—H35 | 0.9500 |
C13—H13B | 0.9800 | C35—C36 | 1.381 (4) |
C13—H13C | 0.9800 | C35—C40 | 1.390 (4) |
C14—C15 | 1.527 (4) | C36—H36 | 0.9500 |
C14—C16 | 1.527 (4) | C36—C37 | 1.367 (5) |
C14—C17 | 1.523 (4) | C37—H37 | 0.9500 |
C15—H15A | 0.9800 | C37—C38 | 1.381 (5) |
C15—H15B | 0.9800 | C38—H38 | 0.9500 |
C15—H15C | 0.9800 | C38—C39 | 1.404 (4) |
C16—H16A | 0.9800 | C39—H39 | 0.9500 |
C16—H16B | 0.9800 | C39—C40 | 1.379 (4) |
O1—Fe1—S1 | 110.51 (6) | C14—C16—H16B | 109.5 |
O1—Fe1—S2 | 113.78 (6) | C14—C16—H16C | 109.5 |
O1—Fe1—S3 | 141.25 (6) | H16A—C16—H16B | 109.5 |
S2—Fe1—S1 | 92.36 (3) | H16A—C16—H16C | 109.5 |
S3—Fe1—S1 | 93.81 (3) | H16B—C16—H16C | 109.5 |
S3—Fe1—S2 | 94.08 (3) | C14—C17—H17A | 109.5 |
C6—B1—C7 | 110.0 (2) | C14—C17—H17B | 109.5 |
C6—B1—C8 | 104.9 (2) | C14—C17—H17C | 109.5 |
C6—B1—C9 | 105.4 (2) | H17A—C17—H17B | 109.5 |
C7—B1—C8 | 111.5 (2) | H17A—C17—H17C | 109.5 |
C9—B1—C7 | 112.4 (2) | H17B—C17—H17C | 109.5 |
C9—B1—C8 | 112.2 (2) | C19—C18—S3 | 111.02 (19) |
C22—O1—Fe1 | 139.39 (17) | C19—C18—C20 | 111.8 (2) |
C7—S1—Fe1 | 104.38 (10) | C19—C18—C21 | 110.6 (2) |
C7—S1—C10 | 106.06 (14) | C20—C18—S3 | 107.86 (19) |
C10—S1—Fe1 | 111.43 (10) | C20—C18—C21 | 109.5 (2) |
C8—S2—Fe1 | 105.28 (10) | C21—C18—S3 | 105.76 (19) |
C8—S2—C14 | 105.79 (13) | C18—C19—H19A | 109.5 |
C14—S2—Fe1 | 115.66 (9) | C18—C19—H19B | 109.5 |
C9—S3—Fe1 | 103.16 (10) | C18—C19—H19C | 109.5 |
C9—S3—C18 | 105.14 (12) | H19A—C19—H19B | 109.5 |
C18—S3—Fe1 | 117.00 (9) | H19A—C19—H19C | 109.5 |
C2—C1—H1 | 118.4 | H19B—C19—H19C | 109.5 |
C2—C1—C6 | 123.3 (3) | C18—C20—H20A | 109.5 |
C6—C1—H1 | 118.4 | C18—C20—H20B | 109.5 |
C1—C2—H2 | 119.9 | C18—C20—H20C | 109.5 |
C3—C2—C1 | 120.3 (3) | H20A—C20—H20B | 109.5 |
C3—C2—H2 | 119.9 | H20A—C20—H20C | 109.5 |
C2—C3—H3 | 120.6 | H20B—C20—H20C | 109.5 |
C2—C3—C4 | 118.8 (3) | C18—C21—H21A | 109.5 |
C4—C3—H3 | 120.6 | C18—C21—H21B | 109.5 |
C3—C4—H4 | 120.1 | C18—C21—H21C | 109.5 |
C5—C4—C3 | 119.8 (3) | H21A—C21—H21B | 109.5 |
C5—C4—H4 | 120.1 | H21A—C21—H21C | 109.5 |
C4—C5—H5 | 118.1 | H21B—C21—H21C | 109.5 |
C4—C5—C6 | 123.7 (3) | O1—C22—C28 | 110.0 (2) |
C6—C5—H5 | 118.1 | O1—C22—C34 | 107.3 (2) |
C1—C6—B1 | 125.6 (3) | O1—C22—C40 | 109.3 (2) |
C1—C6—C5 | 114.1 (3) | C28—C22—C34 | 111.5 (2) |
C5—C6—B1 | 120.3 (2) | C28—C22—C40 | 107.3 (2) |
B1—C7—S1 | 115.79 (19) | C40—C22—C34 | 111.4 (2) |
B1—C7—H7A | 108.3 | C24—C23—H23 | 119.4 |
B1—C7—H7B | 108.3 | C24—C23—C28 | 121.2 (3) |
S1—C7—H7A | 108.3 | C28—C23—H23 | 119.4 |
S1—C7—H7B | 108.3 | C23—C24—H24 | 119.9 |
H7A—C7—H7B | 107.4 | C25—C24—C23 | 120.2 (3) |
B1—C8—S2 | 115.26 (19) | C25—C24—H24 | 119.9 |
B1—C8—H8A | 108.5 | C24—C25—H25 | 120.2 |
B1—C8—H8B | 108.5 | C26—C25—C24 | 119.7 (3) |
S2—C8—H8A | 108.5 | C26—C25—H25 | 120.2 |
S2—C8—H8B | 108.5 | C25—C26—H26 | 120.0 |
H8A—C8—H8B | 107.5 | C25—C26—C27 | 120.1 (3) |
B1—C9—S3 | 117.97 (19) | C27—C26—H26 | 120.0 |
B1—C9—H9A | 107.8 | C26—C27—H27 | 119.3 |
B1—C9—H9B | 107.8 | C26—C27—C28 | 121.4 (3) |
S3—C9—H9A | 107.8 | C28—C27—H27 | 119.3 |
S3—C9—H9B | 107.8 | C23—C28—C22 | 119.5 (2) |
H9A—C9—H9B | 107.1 | C27—C28—C22 | 123.1 (2) |
C11—C10—S1 | 107.6 (2) | C27—C28—C23 | 117.4 (3) |
C12—C10—S1 | 110.9 (2) | C30—C29—H29 | 119.4 |
C12—C10—C11 | 111.7 (3) | C30—C29—C34 | 121.3 (3) |
C13—C10—S1 | 105.3 (2) | C34—C29—H29 | 119.4 |
C13—C10—C11 | 110.2 (3) | C29—C30—H30 | 119.9 |
C13—C10—C12 | 110.9 (3) | C29—C30—C31 | 120.2 (3) |
C10—C11—H11A | 109.5 | C31—C30—H30 | 119.9 |
C10—C11—H11B | 109.5 | C30—C31—H31 | 120.3 |
C10—C11—H11C | 109.5 | C32—C31—C30 | 119.4 (3) |
H11A—C11—H11B | 109.5 | C32—C31—H31 | 120.3 |
H11A—C11—H11C | 109.5 | C31—C32—H32 | 119.6 |
H11B—C11—H11C | 109.5 | C31—C32—C33 | 120.9 (3) |
C10—C12—H12A | 109.5 | C33—C32—H32 | 119.6 |
C10—C12—H12B | 109.5 | C32—C33—H33 | 119.8 |
C10—C12—H12C | 109.5 | C34—C33—C32 | 120.5 (3) |
H12A—C12—H12B | 109.5 | C34—C33—H33 | 119.8 |
H12A—C12—H12C | 109.5 | C29—C34—C22 | 119.3 (2) |
H12B—C12—H12C | 109.5 | C33—C34—C22 | 122.8 (2) |
C10—C13—H13A | 109.5 | C33—C34—C29 | 117.7 (2) |
C10—C13—H13B | 109.5 | C36—C35—H35 | 119.2 |
C10—C13—H13C | 109.5 | C36—C35—C40 | 121.7 (3) |
H13A—C13—H13B | 109.5 | C40—C35—H35 | 119.2 |
H13A—C13—H13C | 109.5 | C35—C36—H36 | 120.3 |
H13B—C13—H13C | 109.5 | C37—C36—C35 | 119.5 (4) |
C15—C14—S2 | 108.2 (2) | C37—C36—H36 | 120.3 |
C16—C14—S2 | 104.61 (19) | C36—C37—H37 | 119.8 |
C16—C14—C15 | 110.2 (2) | C36—C37—C38 | 120.4 (3) |
C17—C14—S2 | 111.7 (2) | C38—C37—H37 | 119.8 |
C17—C14—C15 | 110.5 (2) | C37—C38—H38 | 120.0 |
C17—C14—C16 | 111.4 (2) | C37—C38—C39 | 119.9 (3) |
C14—C15—H15A | 109.5 | C39—C38—H38 | 120.0 |
C14—C15—H15B | 109.5 | C38—C39—H39 | 120.0 |
C14—C15—H15C | 109.5 | C40—C39—C38 | 120.1 (3) |
H15A—C15—H15B | 109.5 | C40—C39—H39 | 120.0 |
H15A—C15—H15C | 109.5 | C35—C40—C22 | 121.0 (3) |
H15B—C15—H15C | 109.5 | C39—C40—C22 | 120.6 (3) |
C14—C16—H16A | 109.5 | C39—C40—C35 | 118.5 (3) |
Fe1—O1—C22—C28 | 53.6 (3) | C8—S2—C14—C17 | 60.4 (2) |
Fe1—O1—C22—C34 | −68.0 (3) | C9—B1—C6—C1 | −119.6 (3) |
Fe1—O1—C22—C40 | 171.16 (19) | C9—B1—C6—C5 | 61.0 (3) |
Fe1—S1—C7—B1 | −34.9 (2) | C9—B1—C7—S1 | −38.3 (3) |
Fe1—S1—C10—C11 | −169.58 (18) | C9—B1—C8—S2 | 86.0 (3) |
Fe1—S1—C10—C12 | −47.1 (2) | C9—S3—C18—C19 | 60.7 (2) |
Fe1—S1—C10—C13 | 72.9 (2) | C9—S3—C18—C20 | −62.2 (2) |
Fe1—S2—C8—B1 | −34.5 (2) | C9—S3—C18—C21 | −179.30 (19) |
Fe1—S2—C14—C15 | −177.56 (17) | C10—S1—C7—B1 | −152.7 (2) |
Fe1—S2—C14—C16 | 65.0 (2) | C14—S2—C8—B1 | −157.4 (2) |
Fe1—S2—C14—C17 | −55.7 (2) | C18—S3—C9—B1 | −157.5 (2) |
Fe1—S3—C9—B1 | −34.4 (2) | C23—C24—C25—C26 | −0.8 (5) |
Fe1—S3—C18—C19 | −53.0 (2) | C24—C23—C28—C22 | 178.8 (3) |
Fe1—S3—C18—C20 | −175.90 (16) | C24—C23—C28—C27 | 1.4 (4) |
Fe1—S3—C18—C21 | 67.0 (2) | C24—C25—C26—C27 | 0.4 (4) |
O1—C22—C28—C23 | 35.2 (3) | C25—C26—C27—C28 | 1.0 (4) |
O1—C22—C28—C27 | −147.5 (2) | C26—C27—C28—C22 | −179.2 (2) |
O1—C22—C34—C29 | 66.6 (3) | C26—C27—C28—C23 | −1.9 (4) |
O1—C22—C34—C33 | −108.6 (3) | C28—C22—C34—C29 | −54.0 (3) |
O1—C22—C40—C35 | −169.9 (3) | C28—C22—C34—C33 | 130.8 (3) |
O1—C22—C40—C39 | 10.2 (4) | C28—C22—C40—C35 | −50.6 (3) |
S1—Fe1—O1—C22 | −135.4 (2) | C28—C22—C40—C39 | 129.4 (3) |
S2—Fe1—O1—C22 | 122.3 (2) | C28—C23—C24—C25 | −0.1 (4) |
S3—Fe1—O1—C22 | −10.1 (3) | C29—C30—C31—C32 | 0.1 (4) |
C1—C2—C3—C4 | 0.2 (5) | C30—C29—C34—C22 | −175.3 (2) |
C2—C1—C6—B1 | 179.7 (3) | C30—C29—C34—C33 | 0.1 (4) |
C2—C1—C6—C5 | −0.9 (5) | C30—C31—C32—C33 | 0.3 (4) |
C2—C3—C4—C5 | −0.9 (5) | C31—C32—C33—C34 | −0.4 (4) |
C3—C4—C5—C6 | 0.7 (5) | C32—C33—C34—C22 | 175.5 (2) |
C4—C5—C6—B1 | 179.6 (3) | C32—C33—C34—C29 | 0.2 (4) |
C4—C5—C6—C1 | 0.2 (4) | C34—C22—C28—C23 | 154.2 (2) |
C6—B1—C7—S1 | −155.3 (2) | C34—C22—C28—C27 | −28.5 (3) |
C6—B1—C8—S2 | −160.15 (19) | C34—C22—C40—C35 | 71.7 (3) |
C6—B1—C9—S3 | −153.2 (2) | C34—C22—C40—C39 | −108.2 (3) |
C6—C1—C2—C3 | 0.7 (5) | C34—C29—C30—C31 | −0.3 (4) |
C7—B1—C6—C1 | 1.7 (4) | C35—C36—C37—C38 | 0.4 (5) |
C7—B1—C6—C5 | −177.7 (3) | C36—C35—C40—C22 | −179.4 (3) |
C7—B1—C8—S2 | −41.2 (3) | C36—C35—C40—C39 | 0.5 (5) |
C7—B1—C9—S3 | 87.1 (3) | C36—C37—C38—C39 | 0.5 (5) |
C7—S1—C10—C11 | −56.6 (2) | C37—C38—C39—C40 | −1.0 (5) |
C7—S1—C10—C12 | 65.8 (2) | C38—C39—C40—C22 | −179.6 (3) |
C7—S1—C10—C13 | −174.1 (2) | C38—C39—C40—C35 | 0.4 (4) |
C8—B1—C6—C1 | 121.7 (3) | C40—C22—C28—C23 | −83.5 (3) |
C8—B1—C6—C5 | −57.7 (3) | C40—C22—C28—C27 | 93.7 (3) |
C8—B1—C7—S1 | 88.8 (3) | C40—C22—C34—C29 | −173.9 (2) |
C8—B1—C9—S3 | −39.6 (3) | C40—C22—C34—C33 | 10.9 (4) |
C8—S2—C14—C15 | −61.5 (2) | C40—C35—C36—C37 | −0.9 (5) |
C8—S2—C14—C16 | −178.95 (19) |
[Fe(C21H38BS3)(C8H9O)] | F(000) = 2464 |
Mr = 574.50 | Dx = 1.214 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 11.4960 (19) Å | Cell parameters from 1011 reflections |
b = 15.036 (2) Å | θ = 2.2–28.3° |
c = 36.375 (6) Å | µ = 0.70 mm−1 |
β = 91.664 (2)° | T = 200 K |
V = 6285.0 (18) Å3 | Block, yellow |
Z = 8 | 0.39 × 0.37 × 0.15 mm |
Bruker APEX diffractometer | 7796 independent reflections |
Radiation source: fine focus sealed tube | 7494 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
Detector resolution: 8.33 pixels mm-1 | θmax = 28.3°, θmin = 2.2° |
ω scans | h = −15→15 |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | k = −20→20 |
Tmin = 0.897, Tmax = 0.904 | l = −48→48 |
42065 measured reflections |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.079 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0276P)2 + 6.6546P] where P = (Fo2 + 2Fc2)/3 |
7796 reflections | (Δ/σ)max < 0.001 |
337 parameters | Δρmax = 0.36 e Å−3 |
44 restraints | Δρmin = −0.33 e Å−3 |
Experimental. Data collection is performed with four batch runs at φ = 0.00 \ (600 frames), at φ = 90.00 \ (600 frames), at φ = 180 \ (600 frames) and at φ = 270 \ (600 frames). Frame width = 0.30 \& in ω. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 | Occ. (<1) | |
Fe1 | 0.75490 (2) | 0.30452 (2) | 0.12057 (2) | 0.02826 (6) | |
B1 | 1.03587 (13) | 0.28478 (10) | 0.15407 (4) | 0.0237 (3) | |
O1A | 0.6034 (3) | 0.3019 (10) | 0.10315 (15) | 0.0491 (16) | 0.68 (3) |
O1B | 0.6130 (11) | 0.342 (2) | 0.1041 (2) | 0.047 (3) | 0.32 (3) |
S1 | 0.91883 (3) | 0.36996 (2) | 0.09061 (2) | 0.02730 (8) | |
S2 | 0.81771 (3) | 0.35490 (2) | 0.18158 (2) | 0.02609 (8) | |
S3 | 0.85446 (3) | 0.16201 (2) | 0.12765 (2) | 0.02750 (8) | |
C1 | 1.04222 (12) | 0.30703 (10) | 0.10947 (4) | 0.0278 (3) | |
H1A | 1.047568 | 0.250202 | 0.095877 | 0.033* | |
H1B | 1.114347 | 0.340988 | 0.105166 | 0.033* | |
C2 | 0.91773 (14) | 0.34983 (12) | 0.04029 (4) | 0.0355 (3) | |
C3 | 0.81878 (17) | 0.40710 (15) | 0.02433 (5) | 0.0490 (4) | |
H3A | 0.816038 | 0.401584 | −0.002531 | 0.073* | |
H3B | 0.832118 | 0.469403 | 0.031141 | 0.073* | |
H3C | 0.744726 | 0.387043 | 0.034123 | 0.073* | |
C4 | 0.89687 (19) | 0.25224 (14) | 0.03119 (5) | 0.0508 (5) | |
H4A | 0.821222 | 0.233886 | 0.040355 | 0.076* | |
H4B | 0.958467 | 0.216079 | 0.042885 | 0.076* | |
H4C | 0.897499 | 0.243906 | 0.004479 | 0.076* | |
C5 | 1.03460 (17) | 0.38174 (16) | 0.02642 (5) | 0.0502 (5) | |
H5A | 1.097210 | 0.345199 | 0.037311 | 0.075* | |
H5B | 1.046675 | 0.444040 | 0.033473 | 0.075* | |
H5C | 1.034956 | 0.376485 | −0.000430 | 0.075* | |
C6 | 0.97380 (12) | 0.36720 (10) | 0.17680 (4) | 0.0286 (3) | |
H6A | 0.988923 | 0.423779 | 0.163872 | 0.034* | |
H6B | 1.010968 | 0.371322 | 0.201639 | 0.034* | |
C7 | 0.76438 (13) | 0.46583 (10) | 0.19550 (4) | 0.0321 (3) | |
C8 | 0.82242 (19) | 0.48898 (13) | 0.23258 (5) | 0.0490 (5) | |
H8A | 0.906467 | 0.495433 | 0.229645 | 0.074* | |
H8B | 0.807688 | 0.441383 | 0.250247 | 0.074* | |
H8C | 0.790333 | 0.544980 | 0.241622 | 0.074* | |
C9 | 0.79117 (17) | 0.53636 (11) | 0.16703 (5) | 0.0422 (4) | |
H9A | 0.758600 | 0.518162 | 0.142999 | 0.063* | |
H9B | 0.875658 | 0.543307 | 0.165522 | 0.063* | |
H9C | 0.756523 | 0.593073 | 0.174225 | 0.063* | |
C10 | 0.63379 (16) | 0.45368 (14) | 0.19952 (6) | 0.0510 (5) | |
H10A | 0.598688 | 0.510588 | 0.206241 | 0.077* | |
H10B | 0.619684 | 0.409689 | 0.218763 | 0.077* | |
H10C | 0.599001 | 0.432967 | 0.176143 | 0.077* | |
C11 | 0.96969 (12) | 0.18804 (9) | 0.16146 (4) | 0.0283 (3) | |
H11A | 0.936068 | 0.189295 | 0.186202 | 0.034* | |
H11B | 1.028465 | 0.139931 | 0.161308 | 0.034* | |
C12 | 0.75918 (13) | 0.07704 (10) | 0.14836 (5) | 0.0327 (3) | |
C13 | 0.67512 (16) | 0.12063 (12) | 0.17426 (6) | 0.0447 (4) | |
H13A | 0.625672 | 0.075011 | 0.185037 | 0.067* | |
H13B | 0.626373 | 0.163448 | 0.160565 | 0.067* | |
H13C | 0.719053 | 0.151568 | 0.193885 | 0.067* | |
C14 | 0.83350 (17) | 0.00776 (12) | 0.16833 (7) | 0.0512 (5) | |
H14A | 0.874070 | 0.035343 | 0.189473 | 0.077* | |
H14B | 0.890697 | −0.016317 | 0.151520 | 0.077* | |
H14C | 0.783694 | −0.040460 | 0.176870 | 0.077* | |
C15 | 0.69459 (18) | 0.03521 (14) | 0.11535 (6) | 0.0543 (5) | |
H15A | 0.635924 | −0.006499 | 0.124035 | 0.081* | |
H15B | 0.750085 | 0.003331 | 0.100214 | 0.081* | |
H15C | 0.656362 | 0.081992 | 0.100646 | 0.081* | |
C16 | 1.27024 (12) | 0.27885 (10) | 0.15145 (4) | 0.0284 (3) | |
H16 | 1.263364 | 0.286512 | 0.125549 | 0.034* | |
C17 | 1.38105 (13) | 0.27215 (11) | 0.16771 (5) | 0.0338 (3) | |
H17 | 1.447681 | 0.276330 | 0.152959 | 0.041* | |
C18 | 1.39448 (14) | 0.25945 (11) | 0.20520 (5) | 0.0366 (3) | |
H18 | 1.469916 | 0.254758 | 0.216399 | 0.044* | |
C19 | 1.29596 (15) | 0.25365 (12) | 0.22623 (4) | 0.0373 (3) | |
H19 | 1.303769 | 0.244509 | 0.252028 | 0.045* | |
C20 | 1.18589 (13) | 0.26119 (11) | 0.20968 (4) | 0.0323 (3) | |
H20 | 1.119767 | 0.256979 | 0.224652 | 0.039* | |
C21 | 1.16844 (12) | 0.27478 (9) | 0.17166 (4) | 0.0245 (3) | |
C22 | 0.51499 (16) | 0.42829 (18) | 0.06741 (5) | 0.0562 (6) | |
C23 | 0.42905 (18) | 0.45175 (18) | 0.04108 (6) | 0.0587 (5) | |
H23 | 0.423636 | 0.511537 | 0.032766 | 0.070* | |
C24 | 0.35223 (18) | 0.38904 (18) | 0.02710 (6) | 0.0601 (6) | |
H24 | 0.294269 | 0.405608 | 0.009255 | 0.072* | |
C25 | 0.35981 (18) | 0.30245 (17) | 0.03908 (5) | 0.0549 (5) | |
H25 | 0.305775 | 0.259903 | 0.029557 | 0.066* | |
C26 | 0.44429 (17) | 0.27566 (17) | 0.06470 (5) | 0.0525 (5) | |
C27 | 0.52365 (15) | 0.33889 (18) | 0.07861 (5) | 0.0525 (5) | |
C28 | 0.5938 (2) | 0.4984 (2) | 0.08373 (8) | 0.0804 (8) | |
H28A | 0.584259 | 0.553740 | 0.069726 | 0.121* | |
H28B | 0.674827 | 0.478437 | 0.082725 | 0.121* | |
H28C | 0.573885 | 0.508831 | 0.109383 | 0.121* | |
C29 | 0.4504 (3) | 0.18006 (19) | 0.07692 (7) | 0.0782 (8) | |
H29A | 0.521150 | 0.152598 | 0.067723 | 0.117* | |
H29B | 0.382034 | 0.147954 | 0.067144 | 0.117* | |
H29C | 0.451872 | 0.177407 | 0.103850 | 0.117* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.02171 (10) | 0.02806 (11) | 0.03483 (12) | −0.00087 (8) | −0.00249 (8) | 0.00048 (8) |
B1 | 0.0205 (7) | 0.0205 (7) | 0.0300 (7) | 0.0001 (5) | −0.0004 (5) | −0.0012 (5) |
O1A | 0.0269 (10) | 0.072 (5) | 0.0478 (13) | −0.0005 (15) | −0.0108 (8) | 0.008 (2) |
O1B | 0.032 (3) | 0.065 (8) | 0.041 (2) | 0.015 (4) | −0.010 (2) | −0.002 (3) |
S1 | 0.02515 (16) | 0.02752 (17) | 0.02910 (17) | −0.00122 (13) | −0.00148 (13) | 0.00359 (13) |
S2 | 0.02428 (16) | 0.02249 (16) | 0.03154 (17) | 0.00197 (12) | 0.00162 (12) | −0.00109 (12) |
S3 | 0.02476 (16) | 0.02193 (16) | 0.03577 (18) | −0.00322 (12) | 0.00020 (13) | −0.00160 (13) |
C1 | 0.0229 (6) | 0.0278 (7) | 0.0325 (7) | −0.0007 (5) | −0.0026 (5) | 0.0016 (5) |
C2 | 0.0350 (8) | 0.0438 (9) | 0.0274 (7) | −0.0002 (7) | −0.0011 (6) | 0.0033 (6) |
C3 | 0.0452 (10) | 0.0640 (12) | 0.0372 (9) | 0.0069 (9) | −0.0076 (7) | 0.0108 (8) |
C4 | 0.0628 (12) | 0.0501 (11) | 0.0389 (9) | −0.0031 (9) | −0.0071 (8) | −0.0085 (8) |
C5 | 0.0415 (10) | 0.0724 (13) | 0.0371 (9) | −0.0049 (9) | 0.0076 (7) | 0.0074 (9) |
C6 | 0.0224 (6) | 0.0264 (7) | 0.0368 (7) | 0.0013 (5) | −0.0015 (5) | −0.0042 (6) |
C7 | 0.0317 (7) | 0.0263 (7) | 0.0382 (8) | 0.0085 (6) | −0.0006 (6) | −0.0045 (6) |
C8 | 0.0617 (12) | 0.0422 (10) | 0.0425 (9) | 0.0150 (9) | −0.0081 (8) | −0.0147 (8) |
C9 | 0.0481 (10) | 0.0265 (8) | 0.0519 (10) | 0.0061 (7) | −0.0026 (8) | 0.0024 (7) |
C10 | 0.0317 (9) | 0.0471 (10) | 0.0746 (13) | 0.0127 (8) | 0.0070 (8) | −0.0032 (9) |
C11 | 0.0240 (6) | 0.0233 (6) | 0.0372 (7) | −0.0009 (5) | −0.0029 (5) | 0.0007 (5) |
C12 | 0.0272 (7) | 0.0223 (7) | 0.0486 (9) | −0.0058 (5) | 0.0026 (6) | 0.0002 (6) |
C13 | 0.0405 (9) | 0.0379 (9) | 0.0566 (11) | −0.0022 (7) | 0.0151 (8) | 0.0027 (8) |
C14 | 0.0417 (10) | 0.0275 (8) | 0.0843 (15) | −0.0011 (7) | 0.0027 (9) | 0.0154 (9) |
C15 | 0.0467 (11) | 0.0486 (11) | 0.0674 (13) | −0.0227 (9) | 0.0002 (9) | −0.0133 (9) |
C16 | 0.0254 (7) | 0.0287 (7) | 0.0312 (7) | 0.0007 (5) | 0.0001 (5) | −0.0003 (5) |
C17 | 0.0241 (7) | 0.0355 (8) | 0.0418 (8) | 0.0004 (6) | 0.0017 (6) | −0.0015 (6) |
C18 | 0.0272 (7) | 0.0384 (8) | 0.0436 (9) | 0.0025 (6) | −0.0095 (6) | −0.0042 (7) |
C19 | 0.0379 (8) | 0.0437 (9) | 0.0299 (7) | 0.0045 (7) | −0.0063 (6) | −0.0013 (6) |
C20 | 0.0284 (7) | 0.0370 (8) | 0.0315 (7) | 0.0036 (6) | 0.0017 (6) | −0.0005 (6) |
C21 | 0.0222 (6) | 0.0194 (6) | 0.0318 (7) | 0.0004 (5) | −0.0014 (5) | −0.0024 (5) |
C22 | 0.0297 (8) | 0.0978 (18) | 0.0413 (10) | 0.0038 (10) | 0.0041 (7) | −0.0106 (11) |
C23 | 0.0412 (10) | 0.0803 (16) | 0.0545 (12) | 0.0105 (10) | 0.0011 (9) | 0.0060 (11) |
C24 | 0.0399 (10) | 0.0956 (18) | 0.0442 (10) | 0.0143 (11) | −0.0126 (8) | 0.0049 (11) |
C25 | 0.0418 (10) | 0.0826 (16) | 0.0399 (10) | 0.0060 (10) | −0.0083 (8) | −0.0067 (10) |
C26 | 0.0424 (10) | 0.0816 (15) | 0.0334 (9) | 0.0212 (10) | 0.0004 (7) | −0.0057 (9) |
C27 | 0.0262 (8) | 0.1018 (17) | 0.0296 (8) | 0.0178 (9) | 0.0001 (6) | −0.0019 (9) |
C28 | 0.0482 (13) | 0.118 (2) | 0.0750 (16) | −0.0107 (14) | 0.0043 (11) | −0.0266 (16) |
C29 | 0.096 (2) | 0.0861 (19) | 0.0518 (13) | 0.0343 (16) | −0.0057 (13) | −0.0055 (12) |
Fe1—O1A | 1.837 (3) | C10—H10B | 0.9800 |
Fe1—O1B | 1.811 (6) | C10—H10C | 0.9800 |
Fe1—S1 | 2.4139 (5) | C11—H11A | 0.9900 |
Fe1—S2 | 2.4344 (5) | C11—H11B | 0.9900 |
Fe1—S3 | 2.4394 (5) | C12—C13 | 1.518 (2) |
B1—C1 | 1.660 (2) | C12—C14 | 1.519 (2) |
B1—C6 | 1.662 (2) | C12—C15 | 1.529 (2) |
B1—C11 | 1.667 (2) | C13—H13A | 0.9800 |
B1—C21 | 1.642 (2) | C13—H13B | 0.9800 |
O1A—O1B | 0.611 (16) | C13—H13C | 0.9800 |
O1A—C27 | 1.378 (5) | C14—H14A | 0.9800 |
O1B—C27 | 1.363 (9) | C14—H14B | 0.9800 |
S1—C1 | 1.8226 (14) | C14—H14C | 0.9800 |
S1—C2 | 1.8547 (16) | C15—H15A | 0.9800 |
S2—C6 | 1.8172 (15) | C15—H15B | 0.9800 |
S2—C7 | 1.8527 (15) | C15—H15C | 0.9800 |
S3—C11 | 1.8236 (15) | C16—H16 | 0.9500 |
S3—C12 | 1.8567 (15) | C16—C17 | 1.393 (2) |
C1—H1A | 0.9900 | C16—C21 | 1.4013 (19) |
C1—H1B | 0.9900 | C17—H17 | 0.9500 |
C2—C3 | 1.528 (2) | C17—C18 | 1.381 (2) |
C2—C4 | 1.522 (3) | C18—H18 | 0.9500 |
C2—C5 | 1.526 (2) | C18—C19 | 1.388 (2) |
C3—H3A | 0.9800 | C19—H19 | 0.9500 |
C3—H3B | 0.9800 | C19—C20 | 1.390 (2) |
C3—H3C | 0.9800 | C20—H20 | 0.9500 |
C4—H4A | 0.9800 | C20—C21 | 1.407 (2) |
C4—H4B | 0.9800 | C22—C23 | 1.401 (3) |
C4—H4C | 0.9800 | C22—C27 | 1.407 (4) |
C5—H5A | 0.9800 | C22—C28 | 1.501 (3) |
C5—H5B | 0.9800 | C23—H23 | 0.9500 |
C5—H5C | 0.9800 | C23—C24 | 1.379 (3) |
C6—H6A | 0.9900 | C24—H24 | 0.9500 |
C6—H6B | 0.9900 | C24—C25 | 1.375 (3) |
C7—C8 | 1.527 (2) | C25—H25 | 0.9500 |
C7—C9 | 1.520 (2) | C25—C26 | 1.386 (3) |
C7—C10 | 1.524 (2) | C26—C27 | 1.402 (3) |
C8—H8A | 0.9800 | C26—C29 | 1.506 (4) |
C8—H8B | 0.9800 | C28—H28A | 0.9800 |
C8—H8C | 0.9800 | C28—H28B | 0.9800 |
C9—H9A | 0.9800 | C28—H28C | 0.9800 |
C9—H9B | 0.9800 | C29—H29A | 0.9800 |
C9—H9C | 0.9800 | C29—H29B | 0.9800 |
C10—H10A | 0.9800 | C29—H29C | 0.9800 |
O1A—Fe1—S1 | 126.73 (18) | C7—C10—H10B | 109.5 |
O1A—Fe1—S2 | 125.1 (3) | C7—C10—H10C | 109.5 |
O1A—Fe1—S3 | 117.1 (5) | H10A—C10—H10B | 109.5 |
C27—O1A—Fe1 | 145.2 (7) | H10A—C10—H10C | 109.5 |
O1B—Fe1—O1A | 19.3 (5) | H10B—C10—H10C | 109.5 |
O1B—Fe1—S1 | 115.6 (8) | B1—C11—S3 | 113.87 (10) |
O1B—Fe1—S2 | 116.5 (4) | B1—C11—H11A | 108.8 |
O1B—Fe1—S3 | 136.3 (10) | B1—C11—H11B | 108.8 |
S1—Fe1—S2 | 94.016 (16) | S3—C11—H11A | 108.8 |
S1—Fe1—S3 | 92.046 (17) | S3—C11—H11B | 108.8 |
S2—Fe1—S3 | 92.937 (15) | H11A—C11—H11B | 107.7 |
C1—B1—C6 | 111.57 (11) | C13—C12—S3 | 110.39 (11) |
C1—B1—C11 | 111.50 (11) | C13—C12—C14 | 111.03 (16) |
C6—B1—C11 | 111.46 (11) | C13—C12—C15 | 111.20 (15) |
C21—B1—C1 | 109.41 (11) | C14—C12—S3 | 109.61 (11) |
C21—B1—C6 | 106.35 (11) | C14—C12—C15 | 110.31 (15) |
C21—B1—C11 | 106.26 (11) | C15—C12—S3 | 104.08 (12) |
O1B—O1A—Fe1 | 78.0 (8) | C12—C13—H13A | 109.5 |
O1B—O1A—C27 | 75.8 (10) | C12—C13—H13B | 109.5 |
O1A—O1B—Fe1 | 82.7 (9) | C12—C13—H13C | 109.5 |
O1A—O1B—C27 | 78.5 (15) | H13A—C13—H13B | 109.5 |
C27—O1B—Fe1 | 150.3 (11) | H13A—C13—H13C | 109.5 |
C1—S1—Fe1 | 103.16 (5) | H13B—C13—H13C | 109.5 |
C1—S1—C2 | 105.64 (7) | C12—C14—H14A | 109.5 |
C2—S1—Fe1 | 113.33 (5) | C12—C14—H14B | 109.5 |
C6—S2—Fe1 | 102.25 (5) | C12—C14—H14C | 109.5 |
C6—S2—C7 | 105.66 (7) | H14A—C14—H14B | 109.5 |
C7—S2—Fe1 | 115.95 (5) | H14A—C14—H14C | 109.5 |
C11—S3—Fe1 | 102.24 (5) | H14B—C14—H14C | 109.5 |
C11—S3—C12 | 107.44 (7) | C12—C15—H15A | 109.5 |
C12—S3—Fe1 | 111.52 (5) | C12—C15—H15B | 109.5 |
B1—C1—S1 | 114.62 (10) | C12—C15—H15C | 109.5 |
B1—C1—H1A | 108.6 | H15A—C15—H15B | 109.5 |
B1—C1—H1B | 108.6 | H15A—C15—H15C | 109.5 |
S1—C1—H1A | 108.6 | H15B—C15—H15C | 109.5 |
S1—C1—H1B | 108.6 | C17—C16—H16 | 118.6 |
H1A—C1—H1B | 107.6 | C17—C16—C21 | 122.79 (14) |
C3—C2—S1 | 105.48 (12) | C21—C16—H16 | 118.6 |
C4—C2—S1 | 111.62 (12) | C16—C17—H17 | 119.9 |
C4—C2—C3 | 110.48 (15) | C18—C17—C16 | 120.28 (15) |
C4—C2—C5 | 111.46 (16) | C18—C17—H17 | 119.9 |
C5—C2—S1 | 107.10 (12) | C17—C18—H18 | 120.5 |
C5—C2—C3 | 110.48 (15) | C17—C18—C19 | 118.90 (14) |
C2—C3—H3A | 109.5 | C19—C18—H18 | 120.5 |
C2—C3—H3B | 109.5 | C18—C19—H19 | 119.9 |
C2—C3—H3C | 109.5 | C18—C19—C20 | 120.22 (15) |
H3A—C3—H3B | 109.5 | C20—C19—H19 | 119.9 |
H3A—C3—H3C | 109.5 | C19—C20—H20 | 118.7 |
H3B—C3—H3C | 109.5 | C19—C20—C21 | 122.67 (14) |
C2—C4—H4A | 109.5 | C21—C20—H20 | 118.7 |
C2—C4—H4B | 109.5 | C16—C21—B1 | 124.84 (13) |
C2—C4—H4C | 109.5 | C16—C21—C20 | 115.13 (13) |
H4A—C4—H4B | 109.5 | C20—C21—B1 | 120.03 (12) |
H4A—C4—H4C | 109.5 | C23—C22—C27 | 118.7 (2) |
H4B—C4—H4C | 109.5 | C23—C22—C28 | 119.9 (3) |
C2—C5—H5A | 109.5 | C27—C22—C28 | 121.3 (2) |
C2—C5—H5B | 109.5 | C22—C23—H23 | 119.6 |
C2—C5—H5C | 109.5 | C24—C23—C22 | 120.7 (2) |
H5A—C5—H5B | 109.5 | C24—C23—H23 | 119.6 |
H5A—C5—H5C | 109.5 | C23—C24—H24 | 120.1 |
H5B—C5—H5C | 109.5 | C25—C24—C23 | 119.78 (19) |
B1—C6—S2 | 114.27 (10) | C25—C24—H24 | 120.1 |
B1—C6—H6A | 108.7 | C24—C25—H25 | 119.2 |
B1—C6—H6B | 108.7 | C24—C25—C26 | 121.7 (2) |
S2—C6—H6A | 108.7 | C26—C25—H25 | 119.2 |
S2—C6—H6B | 108.7 | C25—C26—C27 | 118.8 (2) |
H6A—C6—H6B | 107.6 | C25—C26—C29 | 120.1 (2) |
C8—C7—S2 | 107.89 (11) | C27—C26—C29 | 121.1 (2) |
C9—C7—S2 | 111.51 (11) | O1A—C27—C22 | 127.8 (6) |
C9—C7—C8 | 110.52 (15) | O1A—C27—C26 | 111.9 (6) |
C9—C7—C10 | 111.63 (14) | O1B—C27—O1A | 25.8 (7) |
C10—C7—S2 | 104.66 (12) | O1B—C27—C22 | 102.2 (13) |
C10—C7—C8 | 110.43 (16) | O1B—C27—C26 | 137.4 (13) |
C7—C8—H8A | 109.5 | C26—C27—C22 | 120.23 (17) |
C7—C8—H8B | 109.5 | C22—C28—H28A | 109.5 |
C7—C8—H8C | 109.5 | C22—C28—H28B | 109.5 |
H8A—C8—H8B | 109.5 | C22—C28—H28C | 109.5 |
H8A—C8—H8C | 109.5 | H28A—C28—H28B | 109.5 |
H8B—C8—H8C | 109.5 | H28A—C28—H28C | 109.5 |
C7—C9—H9A | 109.5 | H28B—C28—H28C | 109.5 |
C7—C9—H9B | 109.5 | C26—C29—H29A | 109.5 |
C7—C9—H9C | 109.5 | C26—C29—H29B | 109.5 |
H9A—C9—H9B | 109.5 | C26—C29—H29C | 109.5 |
H9A—C9—H9C | 109.5 | H29A—C29—H29B | 109.5 |
H9B—C9—H9C | 109.5 | H29A—C29—H29C | 109.5 |
C7—C10—H10A | 109.5 | H29B—C29—H29C | 109.5 |
Fe1—O1A—O1B—C27 | 156.9 (4) | C6—B1—C11—S3 | 92.25 (13) |
Fe1—O1A—C27—O1B | −42.3 (9) | C6—B1—C21—C16 | −124.38 (14) |
Fe1—O1A—C27—C22 | −35.8 (17) | C6—B1—C21—C20 | 55.50 (16) |
Fe1—O1A—C27—C26 | 144.9 (14) | C6—S2—C7—C8 | −62.09 (14) |
Fe1—O1B—C27—O1A | 52 (3) | C6—S2—C7—C9 | 59.46 (13) |
Fe1—O1B—C27—C22 | −123 (4) | C6—S2—C7—C10 | −179.70 (12) |
Fe1—O1B—C27—C26 | 62 (4) | C7—S2—C6—B1 | −164.66 (10) |
Fe1—S1—C1—B1 | −40.28 (10) | C11—B1—C1—S1 | 90.48 (12) |
Fe1—S1—C2—C3 | 71.10 (13) | C11—B1—C6—S2 | −33.05 (15) |
Fe1—S1—C2—C4 | −48.92 (14) | C11—B1—C21—C16 | 116.75 (15) |
Fe1—S1—C2—C5 | −171.18 (11) | C11—B1—C21—C20 | −63.36 (16) |
Fe1—S2—C6—B1 | −42.92 (11) | C11—S3—C12—C13 | 80.18 (13) |
Fe1—S2—C7—C8 | −174.51 (11) | C11—S3—C12—C14 | −42.42 (14) |
Fe1—S2—C7—C9 | −52.96 (13) | C11—S3—C12—C15 | −160.41 (12) |
Fe1—S2—C7—C10 | 67.88 (13) | C12—S3—C11—B1 | −160.41 (10) |
Fe1—S3—C11—B1 | −42.92 (10) | C16—C17—C18—C19 | −0.1 (2) |
Fe1—S3—C12—C13 | −31.09 (14) | C17—C16—C21—B1 | 178.40 (13) |
Fe1—S3—C12—C14 | −153.69 (12) | C17—C16—C21—C20 | −1.5 (2) |
Fe1—S3—C12—C15 | 88.32 (12) | C17—C18—C19—C20 | −0.4 (3) |
O1A—Fe1—O1B—C27 | −51 (3) | C18—C19—C20—C21 | 0.0 (3) |
O1A—O1B—C27—C22 | −174.8 (14) | C19—C20—C21—B1 | −178.95 (14) |
O1A—O1B—C27—C26 | 9.8 (19) | C19—C20—C21—C16 | 0.9 (2) |
O1B—Fe1—O1A—C27 | 41.8 (10) | C21—B1—C1—S1 | −152.27 (9) |
O1B—O1A—C27—C22 | 6.5 (18) | C21—B1—C6—S2 | −148.44 (10) |
O1B—O1A—C27—C26 | −172.9 (15) | C21—B1—C11—S3 | −152.30 (10) |
S1—Fe1—O1A—O1B | −59.9 (18) | C21—C16—C17—C18 | 1.1 (2) |
S1—Fe1—O1A—C27 | −18.1 (19) | C22—C23—C24—C25 | 0.0 (3) |
S1—Fe1—O1B—O1A | 129.8 (16) | C23—C22—C27—O1A | 178.0 (4) |
S1—Fe1—O1B—C27 | 79 (4) | C23—C22—C27—O1B | −179.1 (5) |
S2—Fe1—O1A—O1B | 69.2 (14) | C23—C22—C27—C26 | −2.7 (3) |
S2—Fe1—O1A—C27 | 111.0 (13) | C23—C24—C25—C26 | −0.9 (3) |
S2—Fe1—O1B—O1A | −121.2 (12) | C24—C25—C26—C27 | 0.0 (3) |
S2—Fe1—O1B—C27 | −172 (4) | C24—C25—C26—C29 | −179.5 (2) |
S3—Fe1—O1A—O1B | −175.4 (14) | C25—C26—C27—O1A | −178.8 (4) |
S3—Fe1—O1A—C27 | −133.6 (15) | C25—C26—C27—O1B | 176.6 (6) |
S3—Fe1—O1B—O1A | 5.9 (19) | C25—C26—C27—C22 | 1.8 (3) |
S3—Fe1—O1B—C27 | −45 (5) | C27—O1A—O1B—Fe1 | −156.9 (4) |
C1—B1—C6—S2 | 92.32 (12) | C27—C22—C23—C24 | 1.8 (3) |
C1—B1—C11—S3 | −33.15 (14) | C28—C22—C23—C24 | −176.9 (2) |
C1—B1—C21—C16 | −3.75 (18) | C28—C22—C27—O1A | −3.4 (5) |
C1—B1—C21—C20 | 176.13 (13) | C28—C22—C27—O1B | −0.5 (5) |
C1—S1—C2—C3 | −176.67 (12) | C28—C22—C27—C26 | 175.94 (19) |
C1—S1—C2—C4 | 63.31 (14) | C29—C26—C27—O1A | 0.7 (4) |
C1—S1—C2—C5 | −58.95 (14) | C29—C26—C27—O1B | −3.8 (6) |
C2—S1—C1—B1 | −159.47 (10) | C29—C26—C27—C22 | −178.67 (19) |
C6—B1—C1—S1 | −34.87 (14) |
[Fe2(C21H38BS3)2(C6H5O)2]·2C7H8 | Z = 1 |
Mr = 1277.17 | F(000) = 684 |
Triclinic, P1 | Dx = 1.193 Mg m−3 |
a = 10.359 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 13.084 (4) Å | Cell parameters from 1002 reflections |
c = 13.980 (4) Å | θ = 1.9–25.2° |
α = 71.048 (5)° | µ = 0.62 mm−1 |
β = 87.964 (5)° | T = 200 K |
γ = 82.954 (5)° | Plate, yellow |
V = 1778.4 (9) Å3 | 0.24 × 0.19 × 0.07 mm |
Bruker APEXII CCD diffractometer | 8735 independent reflections |
Radiation source: fine focus sealed tube | 5984 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
Detector resolution: 8.33 pixels mm-1 | θmax = 28.3°, θmin = 1.9° |
φ and ω scans | h = −12→13 |
Absorption correction: multi-scan (SADABS; Bruker, 2007) | k = −17→17 |
Tmin = 0.643, Tmax = 0.746 | l = −18→18 |
19673 measured reflections |
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)] = 0.070 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.199 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0938P)2 + 0.6253P] where P = (Fo2 + 2Fc2)/3 |
8735 reflections | (Δ/σ)max < 0.001 |
400 parameters | Δρmax = 0.93 e Å−3 |
180 restraints | Δρmin = −0.68 e Å−3 |
Experimental. Data collection is performed with four batch runs at φ = 0.00 \ (600 frames), at φ = 90.00 \ (600 frames), at φ = 180 \ (600 frames) and at φ = 270 \ (600 frames). Frame width = 0.30 \& in ω. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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 | Occ. (<1) | |
Fe1 | 0.89498 (5) | 0.20603 (4) | 0.50440 (4) | 0.02994 (16) | |
S1 | 1.12334 (9) | 0.18847 (7) | 0.53288 (7) | 0.0289 (2) | |
S2 | 0.87301 (8) | 0.02926 (7) | 0.62231 (7) | 0.0284 (2) | |
S3 | 1.12005 (9) | −0.20049 (7) | 0.66813 (7) | 0.0298 (2) | |
O1 | 0.7973 (3) | 0.3232 (2) | 0.5298 (2) | 0.0491 (8) | |
C1 | 1.3314 (4) | −0.0441 (3) | 0.8362 (3) | 0.0384 (9) | |
H1 | 1.379157 | −0.025530 | 0.774898 | 0.046* | |
C2 | 1.3992 (4) | −0.0772 (4) | 0.9264 (3) | 0.0460 (10) | |
H2 | 1.491356 | −0.080296 | 0.926369 | 0.055* | |
C3 | 1.3326 (5) | −0.1056 (4) | 1.0164 (3) | 0.0514 (12) | |
H3 | 1.378133 | −0.129067 | 1.079065 | 0.062* | |
C4 | 1.1994 (5) | −0.0997 (4) | 1.0145 (3) | 0.0502 (11) | |
H4 | 1.152923 | −0.120078 | 1.076357 | 0.060* | |
C5 | 1.1314 (4) | −0.0643 (4) | 0.9234 (3) | 0.0388 (9) | |
H5 | 1.039095 | −0.058724 | 0.924332 | 0.047* | |
C6 | 1.1956 (4) | −0.0367 (3) | 0.8307 (3) | 0.0313 (8) | |
C7 | 1.1618 (4) | 0.1295 (3) | 0.6664 (3) | 0.0324 (8) | |
H7A | 1.256274 | 0.128761 | 0.675454 | 0.039* | |
H7B | 1.115693 | 0.177029 | 0.702318 | 0.039* | |
C8 | 1.1871 (4) | 0.3227 (3) | 0.4899 (3) | 0.0373 (9) | |
C9 | 1.1457 (5) | 0.3880 (4) | 0.5599 (4) | 0.0519 (12) | |
H9A | 1.171856 | 0.461272 | 0.531042 | 0.078* | |
H9B | 1.187604 | 0.351959 | 0.626074 | 0.078* | |
H9C | 1.051042 | 0.392923 | 0.567964 | 0.078* | |
C10 | 1.1330 (5) | 0.3790 (4) | 0.3852 (3) | 0.0518 (12) | |
H10A | 1.168860 | 0.448345 | 0.355880 | 0.078* | |
H10B | 1.038021 | 0.392490 | 0.388432 | 0.078* | |
H10C | 1.156806 | 0.332770 | 0.342905 | 0.078* | |
C11 | 1.3358 (4) | 0.2999 (4) | 0.4860 (4) | 0.0601 (14) | |
H11A | 1.372946 | 0.368906 | 0.458443 | 0.090* | |
H11B | 1.359437 | 0.254911 | 0.442598 | 0.090* | |
H11C | 1.369874 | 0.261387 | 0.554378 | 0.090* | |
C12 | 0.9660 (3) | 0.0029 (3) | 0.7370 (3) | 0.0307 (8) | |
H12A | 0.933769 | 0.058412 | 0.769034 | 0.037* | |
H12B | 0.949596 | −0.068943 | 0.784521 | 0.037* | |
C13 | 0.7034 (4) | 0.0070 (3) | 0.6659 (3) | 0.0326 (8) | |
C14 | 0.7018 (5) | −0.1137 (4) | 0.7198 (5) | 0.0621 (14) | |
H14A | 0.613224 | −0.127997 | 0.742404 | 0.093* | |
H14B | 0.760317 | −0.137076 | 0.778463 | 0.093* | |
H14C | 0.730883 | −0.154031 | 0.673364 | 0.093* | |
C15 | 0.6596 (5) | 0.0711 (4) | 0.7362 (4) | 0.0567 (13) | |
H15A | 0.568204 | 0.063169 | 0.753976 | 0.085* | |
H15B | 0.669218 | 0.148096 | 0.702349 | 0.085* | |
H15C | 0.713101 | 0.043537 | 0.797706 | 0.085* | |
C16 | 0.6192 (5) | 0.0440 (6) | 0.5731 (4) | 0.0736 (19) | |
H16A | 0.527976 | 0.038421 | 0.592951 | 0.110* | |
H16B | 0.644755 | −0.001933 | 0.530890 | 0.110* | |
H16C | 0.629787 | 0.119863 | 0.534761 | 0.110* | |
C17 | 1.1818 (4) | −0.0692 (3) | 0.6490 (3) | 0.0284 (7) | |
H17A | 1.277336 | −0.083510 | 0.658808 | 0.034* | |
H17B | 1.165519 | −0.024042 | 0.577497 | 0.034* | |
C18 | 1.2476 (4) | −0.3120 (3) | 0.7368 (3) | 0.0374 (9) | |
C19 | 1.3785 (4) | −0.2994 (4) | 0.6850 (4) | 0.0548 (12) | |
H19A | 1.442138 | −0.360230 | 0.721620 | 0.082* | |
H19B | 1.407478 | −0.230749 | 0.684526 | 0.082* | |
H19C | 1.370437 | −0.299224 | 0.615279 | 0.082* | |
C20 | 1.1982 (5) | −0.4166 (3) | 0.7354 (4) | 0.0511 (11) | |
H20A | 1.259959 | −0.479196 | 0.771555 | 0.077* | |
H20B | 1.189666 | −0.414767 | 0.665274 | 0.077* | |
H20C | 1.113228 | −0.423124 | 0.768556 | 0.077* | |
C21 | 1.2548 (6) | −0.3115 (4) | 0.8455 (3) | 0.0591 (13) | |
H21A | 1.314911 | −0.373758 | 0.884614 | 0.089* | |
H21B | 1.168157 | −0.316529 | 0.875931 | 0.089* | |
H21C | 1.286033 | −0.243834 | 0.845790 | 0.089* | |
C22 | 0.8046 (5) | 0.3260 (4) | 0.6993 (4) | 0.0523 (12) | |
H22 | 0.893664 | 0.296655 | 0.706652 | 0.063* | |
C23 | 0.7385 (8) | 0.3501 (5) | 0.7790 (4) | 0.079 (2) | |
H23 | 0.782365 | 0.336256 | 0.841256 | 0.095* | |
C24 | 0.6099 (9) | 0.3940 (5) | 0.7685 (6) | 0.090 (2) | |
H24 | 0.565521 | 0.411561 | 0.822806 | 0.108* | |
C25 | 0.5465 (7) | 0.4121 (5) | 0.6793 (6) | 0.082 (2) | |
H25 | 0.457335 | 0.440900 | 0.671988 | 0.099* | |
C26 | 0.6109 (5) | 0.3889 (4) | 0.6011 (4) | 0.0530 (12) | |
H26 | 0.566031 | 0.403181 | 0.539131 | 0.064* | |
C27 | 0.7403 (4) | 0.3448 (3) | 0.6094 (3) | 0.0396 (9) | |
B1 | 1.1233 (4) | 0.0039 (3) | 0.7205 (3) | 0.0280 (8) | |
C28A | 0.6605 (9) | −0.3043 (9) | 1.0238 (8) | 0.130 (2) | 0.651 (7) |
H28A | 0.596892 | −0.270854 | 1.058283 | 0.156* | 0.651 (7) |
C29A | 0.6224 (8) | −0.3591 (10) | 0.9614 (8) | 0.131 (2) | 0.651 (7) |
H29A | 0.532755 | −0.363189 | 0.953245 | 0.157* | 0.651 (7) |
C30A | 0.7156 (11) | −0.4080 (9) | 0.9109 (8) | 0.1310 (19) | 0.651 (7) |
H30A | 0.689547 | −0.445526 | 0.868242 | 0.157* | 0.651 (7) |
C31A | 0.8468 (10) | −0.4021 (9) | 0.9228 (7) | 0.131 (2) | 0.651 (7) |
H31A | 0.910476 | −0.435529 | 0.888276 | 0.157* | 0.651 (7) |
C32A | 0.8849 (8) | −0.3473 (9) | 0.9852 (8) | 0.131 (2) | 0.651 (7) |
H32A | 0.974616 | −0.343194 | 0.993313 | 0.157* | 0.651 (7) |
C33A | 0.7918 (10) | −0.2983 (9) | 1.0357 (7) | 0.130 (2) | 0.651 (7) |
C34A | 0.8343 (14) | −0.2534 (13) | 1.1104 (11) | 0.138 (3) | 0.651 (7) |
H34A | 0.928387 | −0.250309 | 1.104726 | 0.208* | 0.651 (7) |
H34B | 0.813592 | −0.299724 | 1.178366 | 0.208* | 0.651 (7) |
H34C | 0.789374 | −0.179830 | 1.098200 | 0.208* | 0.651 (7) |
C32B | 0.8687 (16) | −0.3485 (16) | 0.9708 (14) | 0.131 (2) | 0.349 (7) |
H32B | 0.918915 | −0.387646 | 0.932990 | 0.157* | 0.349 (7) |
C31B | 0.9286 (15) | −0.2870 (17) | 1.0167 (14) | 0.131 (2) | 0.349 (7) |
H31B | 1.019792 | −0.284065 | 1.010301 | 0.157* | 0.349 (7) |
C30B | 0.855 (2) | −0.2298 (15) | 1.0720 (13) | 0.1310 (19) | 0.349 (7) |
H30B | 0.896040 | −0.187712 | 1.103367 | 0.157* | 0.349 (7) |
C29B | 0.722 (2) | −0.2341 (15) | 1.0813 (13) | 0.131 (2) | 0.349 (7) |
H29B | 0.671411 | −0.194939 | 1.119123 | 0.157* | 0.349 (7) |
C28B | 0.6617 (14) | −0.2956 (16) | 1.0354 (15) | 0.131 (2) | 0.349 (7) |
H28B | 0.570532 | −0.298518 | 1.041813 | 0.157* | 0.349 (7) |
C33B | 0.7352 (16) | −0.3528 (15) | 0.9801 (15) | 0.131 (2) | 0.349 (7) |
C34B | 0.670 (2) | −0.400 (3) | 0.918 (2) | 0.1310 (19) | 0.349 (7) |
H34D | 0.733096 | −0.422222 | 0.872577 | 0.196* | 0.349 (7) |
H34E | 0.601558 | −0.346367 | 0.878413 | 0.196* | 0.349 (7) |
H34F | 0.631525 | −0.463900 | 0.961634 | 0.196* | 0.349 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0274 (3) | 0.0293 (3) | 0.0345 (3) | −0.0026 (2) | −0.0021 (2) | −0.0122 (2) |
S1 | 0.0287 (5) | 0.0258 (4) | 0.0327 (5) | −0.0066 (3) | −0.0006 (3) | −0.0088 (3) |
S2 | 0.0226 (4) | 0.0352 (5) | 0.0284 (4) | −0.0063 (3) | 0.0010 (3) | −0.0105 (4) |
S3 | 0.0292 (5) | 0.0278 (4) | 0.0314 (5) | −0.0025 (4) | −0.0023 (3) | −0.0085 (3) |
O1 | 0.056 (2) | 0.0390 (16) | 0.0530 (19) | 0.0044 (14) | 0.0024 (15) | −0.0202 (14) |
C1 | 0.033 (2) | 0.048 (2) | 0.036 (2) | −0.0088 (18) | −0.0013 (16) | −0.0134 (18) |
C2 | 0.038 (2) | 0.058 (3) | 0.040 (2) | −0.003 (2) | −0.0113 (18) | −0.013 (2) |
C3 | 0.052 (3) | 0.065 (3) | 0.035 (2) | 0.005 (2) | −0.0146 (19) | −0.017 (2) |
C4 | 0.048 (3) | 0.069 (3) | 0.030 (2) | 0.005 (2) | −0.0003 (18) | −0.016 (2) |
C5 | 0.032 (2) | 0.051 (2) | 0.032 (2) | 0.0002 (18) | 0.0003 (16) | −0.0140 (18) |
C6 | 0.0310 (19) | 0.0326 (19) | 0.0307 (18) | −0.0032 (15) | −0.0022 (15) | −0.0108 (15) |
C7 | 0.034 (2) | 0.0335 (19) | 0.0322 (19) | −0.0067 (16) | −0.0050 (15) | −0.0123 (15) |
C8 | 0.035 (2) | 0.0255 (18) | 0.051 (2) | −0.0087 (16) | −0.0004 (18) | −0.0114 (17) |
C9 | 0.067 (3) | 0.036 (2) | 0.056 (3) | −0.015 (2) | −0.001 (2) | −0.016 (2) |
C10 | 0.066 (3) | 0.036 (2) | 0.050 (3) | −0.019 (2) | 0.003 (2) | −0.0062 (19) |
C11 | 0.038 (3) | 0.050 (3) | 0.093 (4) | −0.020 (2) | 0.010 (3) | −0.018 (3) |
C12 | 0.0255 (18) | 0.039 (2) | 0.0283 (18) | −0.0028 (15) | −0.0017 (14) | −0.0128 (15) |
C13 | 0.0220 (18) | 0.041 (2) | 0.037 (2) | −0.0089 (15) | 0.0047 (14) | −0.0143 (16) |
C14 | 0.046 (3) | 0.047 (3) | 0.093 (4) | −0.022 (2) | 0.021 (3) | −0.018 (3) |
C15 | 0.040 (3) | 0.068 (3) | 0.081 (4) | −0.022 (2) | 0.026 (2) | −0.046 (3) |
C16 | 0.026 (2) | 0.142 (6) | 0.045 (3) | −0.022 (3) | −0.0002 (19) | −0.015 (3) |
C17 | 0.0275 (18) | 0.0262 (17) | 0.0316 (18) | −0.0042 (14) | −0.0004 (14) | −0.0090 (14) |
C18 | 0.040 (2) | 0.0261 (18) | 0.042 (2) | 0.0016 (16) | −0.0097 (17) | −0.0073 (16) |
C19 | 0.035 (2) | 0.045 (3) | 0.079 (4) | 0.007 (2) | −0.007 (2) | −0.015 (2) |
C20 | 0.056 (3) | 0.031 (2) | 0.061 (3) | −0.001 (2) | −0.012 (2) | −0.008 (2) |
C21 | 0.077 (4) | 0.050 (3) | 0.043 (3) | 0.006 (3) | −0.022 (2) | −0.007 (2) |
C22 | 0.062 (3) | 0.037 (2) | 0.059 (3) | −0.011 (2) | −0.004 (2) | −0.014 (2) |
C23 | 0.138 (7) | 0.056 (3) | 0.047 (3) | −0.034 (4) | 0.006 (4) | −0.014 (3) |
C24 | 0.124 (7) | 0.060 (4) | 0.091 (5) | −0.021 (4) | 0.062 (5) | −0.033 (4) |
C25 | 0.068 (4) | 0.059 (4) | 0.116 (6) | −0.008 (3) | 0.035 (4) | −0.028 (4) |
C26 | 0.042 (3) | 0.044 (3) | 0.075 (3) | −0.002 (2) | 0.001 (2) | −0.024 (2) |
C27 | 0.040 (2) | 0.0289 (19) | 0.052 (2) | −0.0050 (17) | 0.0057 (19) | −0.0156 (18) |
B1 | 0.026 (2) | 0.031 (2) | 0.0269 (19) | −0.0049 (16) | −0.0004 (15) | −0.0100 (16) |
C28A | 0.143 (4) | 0.123 (4) | 0.104 (4) | −0.015 (4) | 0.005 (3) | −0.008 (3) |
C29A | 0.142 (4) | 0.124 (4) | 0.105 (4) | −0.016 (4) | 0.003 (3) | −0.007 (3) |
C30A | 0.143 (4) | 0.124 (4) | 0.106 (4) | −0.016 (4) | 0.003 (3) | −0.010 (3) |
C31A | 0.144 (4) | 0.125 (4) | 0.105 (4) | −0.015 (4) | 0.006 (3) | −0.012 (3) |
C32A | 0.144 (4) | 0.125 (4) | 0.106 (4) | −0.017 (4) | 0.005 (3) | −0.011 (3) |
C33A | 0.146 (4) | 0.123 (4) | 0.103 (4) | −0.018 (4) | 0.004 (3) | −0.012 (3) |
C34A | 0.162 (6) | 0.128 (5) | 0.110 (5) | −0.024 (5) | −0.003 (5) | −0.015 (4) |
C32B | 0.141 (5) | 0.125 (5) | 0.107 (4) | −0.016 (4) | 0.003 (4) | −0.009 (3) |
C31B | 0.142 (5) | 0.124 (4) | 0.107 (4) | −0.016 (4) | 0.004 (4) | −0.010 (3) |
C30B | 0.143 (4) | 0.124 (4) | 0.106 (4) | −0.016 (4) | 0.003 (3) | −0.010 (3) |
C29B | 0.142 (5) | 0.124 (4) | 0.106 (4) | −0.015 (4) | 0.003 (4) | −0.008 (3) |
C28B | 0.141 (5) | 0.124 (5) | 0.106 (4) | −0.015 (4) | 0.003 (4) | −0.007 (3) |
C33B | 0.142 (5) | 0.124 (5) | 0.106 (4) | −0.016 (4) | 0.002 (4) | −0.008 (3) |
C34B | 0.143 (4) | 0.124 (4) | 0.106 (4) | −0.016 (4) | 0.003 (3) | −0.010 (3) |
Fe1—O1 | 1.857 (3) | C17—B1 | 1.649 (5) |
Fe1—S1 | 2.3834 (12) | C18—C19 | 1.515 (6) |
Fe1—S2 | 2.3968 (12) | C18—C20 | 1.525 (6) |
Fe1—S3i | 2.4475 (13) | C18—C21 | 1.526 (6) |
S1—C7 | 1.811 (4) | C19—H19A | 0.9800 |
S1—C8 | 1.857 (4) | C19—H19B | 0.9800 |
S2—C12 | 1.812 (4) | C19—H19C | 0.9800 |
S2—C13 | 1.865 (4) | C20—H20A | 0.9800 |
S3—C17 | 1.841 (4) | C20—H20B | 0.9800 |
S3—C18 | 1.872 (4) | C20—H20C | 0.9800 |
O1—C27 | 1.335 (5) | C21—H21A | 0.9800 |
C1—H1 | 0.9500 | C21—H21B | 0.9800 |
C1—C2 | 1.380 (5) | C21—H21C | 0.9800 |
C1—C6 | 1.401 (5) | C22—H22 | 0.9500 |
C2—H2 | 0.9500 | C22—C23 | 1.391 (8) |
C2—C3 | 1.377 (6) | C22—C27 | 1.378 (6) |
C3—H3 | 0.9500 | C23—H23 | 0.9500 |
C3—C4 | 1.373 (7) | C23—C24 | 1.377 (10) |
C4—H4 | 0.9500 | C24—H24 | 0.9500 |
C4—C5 | 1.390 (6) | C24—C25 | 1.368 (10) |
C5—H5 | 0.9500 | C25—H25 | 0.9500 |
C5—C6 | 1.396 (5) | C25—C26 | 1.359 (8) |
C6—B1 | 1.634 (5) | C26—H26 | 0.9500 |
C7—H7A | 0.9900 | C26—C27 | 1.386 (6) |
C7—H7B | 0.9900 | C28A—H28A | 0.9500 |
C7—B1 | 1.662 (5) | C28A—C29A | 1.3900 |
C8—C9 | 1.515 (6) | C28A—C33A | 1.3900 |
C8—C10 | 1.502 (6) | C29A—H29A | 0.9500 |
C8—C11 | 1.535 (6) | C29A—C30A | 1.3900 |
C9—H9A | 0.9800 | C30A—H30A | 0.9500 |
C9—H9B | 0.9800 | C30A—C31A | 1.3900 |
C9—H9C | 0.9800 | C31A—H31A | 0.9500 |
C10—H10A | 0.9800 | C31A—C32A | 1.3900 |
C10—H10B | 0.9800 | C32A—H32A | 0.9500 |
C10—H10C | 0.9800 | C32A—C33A | 1.3900 |
C11—H11A | 0.9800 | C33A—C34A | 1.458 (14) |
C11—H11B | 0.9800 | C34A—H34A | 0.9800 |
C11—H11C | 0.9800 | C34A—H34B | 0.9800 |
C12—H12A | 0.9900 | C34A—H34C | 0.9800 |
C12—H12B | 0.9900 | C32B—H32B | 0.9500 |
C12—B1 | 1.639 (5) | C32B—C31B | 1.3900 |
C13—C14 | 1.514 (6) | C32B—C33B | 1.3900 |
C13—C15 | 1.511 (6) | C31B—H31B | 0.9500 |
C13—C16 | 1.499 (6) | C31B—C30B | 1.3900 |
C14—H14A | 0.9800 | C30B—H30B | 0.9500 |
C14—H14B | 0.9800 | C30B—C29B | 1.3900 |
C14—H14C | 0.9800 | C29B—H29B | 0.9500 |
C15—H15A | 0.9800 | C29B—C28B | 1.3900 |
C15—H15B | 0.9800 | C28B—H28B | 0.9500 |
C15—H15C | 0.9800 | C28B—C33B | 1.3900 |
C16—H16A | 0.9800 | C33B—C34B | 1.441 (17) |
C16—H16B | 0.9800 | C34B—H34D | 0.9800 |
C16—H16C | 0.9800 | C34B—H34E | 0.9800 |
C17—H17A | 0.9900 | C34B—H34F | 0.9800 |
C17—H17B | 0.9900 | ||
S1—Fe1—S2 | 93.03 (4) | B1—C17—H17A | 107.7 |
S1—Fe1—S3i | 103.51 (4) | B1—C17—H17B | 107.7 |
S2—Fe1—S3i | 109.35 (4) | C19—C18—S3 | 111.6 (3) |
O1—Fe1—S1 | 116.06 (11) | C19—C18—C20 | 110.5 (4) |
O1—Fe1—S2 | 116.61 (11) | C19—C18—C21 | 111.5 (4) |
O1—Fe1—S3i | 115.48 (10) | C20—C18—S3 | 104.9 (3) |
C7—S1—Fe1 | 111.05 (13) | C20—C18—C21 | 109.9 (4) |
C7—S1—C8 | 106.23 (18) | C21—C18—S3 | 108.2 (3) |
C8—S1—Fe1 | 111.75 (13) | C18—C19—H19A | 109.5 |
C12—S2—Fe1 | 111.77 (13) | C18—C19—H19B | 109.5 |
C12—S2—C13 | 104.97 (17) | C18—C19—H19C | 109.5 |
C13—S2—Fe1 | 114.64 (13) | H19A—C19—H19B | 109.5 |
C17—S3—Fe1i | 102.94 (12) | H19A—C19—H19C | 109.5 |
C17—S3—C18 | 108.29 (17) | H19B—C19—H19C | 109.5 |
C18—S3—Fe1i | 107.77 (13) | C18—C20—H20A | 109.5 |
C27—O1—Fe1 | 137.2 (3) | C18—C20—H20B | 109.5 |
C2—C1—H1 | 118.4 | C18—C20—H20C | 109.5 |
C2—C1—C6 | 123.2 (4) | H20A—C20—H20B | 109.5 |
C6—C1—H1 | 118.4 | H20A—C20—H20C | 109.5 |
C1—C2—H2 | 120.2 | H20B—C20—H20C | 109.5 |
C3—C2—C1 | 119.6 (4) | C18—C21—H21A | 109.5 |
C3—C2—H2 | 120.2 | C18—C21—H21B | 109.5 |
C2—C3—H3 | 120.4 | C18—C21—H21C | 109.5 |
C4—C3—C2 | 119.1 (4) | H21A—C21—H21B | 109.5 |
C4—C3—H3 | 120.4 | H21A—C21—H21C | 109.5 |
C3—C4—H4 | 119.5 | H21B—C21—H21C | 109.5 |
C3—C4—C5 | 121.0 (4) | C23—C22—H22 | 120.2 |
C5—C4—H4 | 119.5 | C27—C22—H22 | 120.2 |
C4—C5—H5 | 119.2 | C27—C22—C23 | 119.6 (5) |
C4—C5—C6 | 121.5 (4) | C22—C23—H23 | 119.7 |
C6—C5—H5 | 119.2 | C24—C23—C22 | 120.6 (6) |
C1—C6—B1 | 119.9 (3) | C24—C23—H23 | 119.7 |
C5—C6—C1 | 115.5 (3) | C23—C24—H24 | 120.3 |
C5—C6—B1 | 124.6 (3) | C25—C24—C23 | 119.5 (6) |
S1—C7—H7A | 108.5 | C25—C24—H24 | 120.3 |
S1—C7—H7B | 108.5 | C24—C25—H25 | 119.9 |
H7A—C7—H7B | 107.5 | C26—C25—C24 | 120.2 (6) |
B1—C7—S1 | 115.1 (2) | C26—C25—H25 | 119.9 |
B1—C7—H7A | 108.5 | C25—C26—H26 | 119.2 |
B1—C7—H7B | 108.5 | C25—C26—C27 | 121.6 (6) |
C9—C8—S1 | 111.5 (3) | C27—C26—H26 | 119.2 |
C9—C8—C11 | 111.3 (4) | O1—C27—C22 | 123.0 (4) |
C10—C8—S1 | 105.4 (3) | O1—C27—C26 | 118.5 (4) |
C10—C8—C9 | 111.4 (4) | C22—C27—C26 | 118.5 (4) |
C10—C8—C11 | 110.1 (4) | C6—B1—C7 | 104.0 (3) |
C11—C8—S1 | 106.9 (3) | C6—B1—C12 | 109.3 (3) |
C8—C9—H9A | 109.5 | C6—B1—C17 | 111.9 (3) |
C8—C9—H9B | 109.5 | C12—B1—C7 | 111.6 (3) |
C8—C9—H9C | 109.5 | C12—B1—C17 | 112.2 (3) |
H9A—C9—H9B | 109.5 | C17—B1—C7 | 107.6 (3) |
H9A—C9—H9C | 109.5 | C29A—C28A—H28A | 120.0 |
H9B—C9—H9C | 109.5 | C29A—C28A—C33A | 120.0 |
C8—C10—H10A | 109.5 | C33A—C28A—H28A | 120.0 |
C8—C10—H10B | 109.5 | C28A—C29A—H29A | 120.0 |
C8—C10—H10C | 109.5 | C30A—C29A—C28A | 120.0 |
H10A—C10—H10B | 109.5 | C30A—C29A—H29A | 120.0 |
H10A—C10—H10C | 109.5 | C29A—C30A—H30A | 120.0 |
H10B—C10—H10C | 109.5 | C31A—C30A—C29A | 120.0 |
C8—C11—H11A | 109.5 | C31A—C30A—H30A | 120.0 |
C8—C11—H11B | 109.5 | C30A—C31A—H31A | 120.0 |
C8—C11—H11C | 109.5 | C30A—C31A—C32A | 120.0 |
H11A—C11—H11B | 109.5 | C32A—C31A—H31A | 120.0 |
H11A—C11—H11C | 109.5 | C31A—C32A—H32A | 120.0 |
H11B—C11—H11C | 109.5 | C33A—C32A—C31A | 120.0 |
S2—C12—H12A | 108.6 | C33A—C32A—H32A | 120.0 |
S2—C12—H12B | 108.6 | C28A—C33A—C34A | 120.6 (7) |
H12A—C12—H12B | 107.6 | C32A—C33A—C28A | 120.0 |
B1—C12—S2 | 114.8 (2) | C32A—C33A—C34A | 119.0 (7) |
B1—C12—H12A | 108.6 | C33A—C34A—H34A | 109.5 |
B1—C12—H12B | 108.6 | C33A—C34A—H34B | 109.5 |
C14—C13—S2 | 107.7 (3) | C33A—C34A—H34C | 109.5 |
C15—C13—S2 | 110.5 (3) | H34A—C34A—H34B | 109.5 |
C15—C13—C14 | 110.5 (4) | H34A—C34A—H34C | 109.5 |
C16—C13—S2 | 106.8 (3) | H34B—C34A—H34C | 109.5 |
C16—C13—C14 | 110.6 (4) | C31B—C32B—H32B | 120.0 |
C16—C13—C15 | 110.6 (4) | C31B—C32B—C33B | 120.0 |
C13—C14—H14A | 109.5 | C33B—C32B—H32B | 120.0 |
C13—C14—H14B | 109.5 | C32B—C31B—H31B | 120.0 |
C13—C14—H14C | 109.5 | C32B—C31B—C30B | 120.0 |
H14A—C14—H14B | 109.5 | C30B—C31B—H31B | 120.0 |
H14A—C14—H14C | 109.5 | C31B—C30B—H30B | 120.0 |
H14B—C14—H14C | 109.5 | C29B—C30B—C31B | 120.0 |
C13—C15—H15A | 109.5 | C29B—C30B—H30B | 120.0 |
C13—C15—H15B | 109.5 | C30B—C29B—H29B | 120.0 |
C13—C15—H15C | 109.5 | C30B—C29B—C28B | 120.0 |
H15A—C15—H15B | 109.5 | C28B—C29B—H29B | 120.0 |
H15A—C15—H15C | 109.5 | C29B—C28B—H28B | 120.0 |
H15B—C15—H15C | 109.5 | C33B—C28B—C29B | 120.0 |
C13—C16—H16A | 109.5 | C33B—C28B—H28B | 120.0 |
C13—C16—H16B | 109.5 | C32B—C33B—C34B | 119.7 (8) |
C13—C16—H16C | 109.5 | C28B—C33B—C32B | 120.0 |
H16A—C16—H16B | 109.5 | C28B—C33B—C34B | 119.4 (8) |
H16A—C16—H16C | 109.5 | C33B—C34B—H34D | 109.5 |
H16B—C16—H16C | 109.5 | C33B—C34B—H34E | 109.5 |
S3—C17—H17A | 107.7 | C33B—C34B—H34F | 109.5 |
S3—C17—H17B | 107.7 | H34D—C34B—H34E | 109.5 |
H17A—C17—H17B | 107.1 | H34D—C34B—H34F | 109.5 |
B1—C17—S3 | 118.3 (2) | H34E—C34B—H34F | 109.5 |
Fe1—S1—C7—B1 | 62.5 (3) | C5—C6—B1—C17 | −126.7 (4) |
Fe1—S1—C8—C9 | 72.6 (3) | C6—C1—C2—C3 | 0.6 (7) |
Fe1—S1—C8—C10 | −48.5 (3) | C7—S1—C8—C9 | −48.7 (4) |
Fe1—S1—C8—C11 | −165.6 (3) | C7—S1—C8—C10 | −169.7 (3) |
Fe1—S2—C12—B1 | −61.6 (3) | C7—S1—C8—C11 | 73.2 (4) |
Fe1—S2—C13—C14 | 167.4 (3) | C8—S1—C7—B1 | −175.8 (3) |
Fe1—S2—C13—C15 | −71.8 (3) | C12—S2—C13—C14 | −69.5 (3) |
Fe1—S2—C13—C16 | 48.6 (4) | C12—S2—C13—C15 | 51.3 (4) |
Fe1i—S3—C17—B1 | 141.1 (2) | C12—S2—C13—C16 | 171.7 (4) |
Fe1i—S3—C18—C19 | 58.7 (3) | C13—S2—C12—B1 | 173.6 (3) |
Fe1i—S3—C18—C20 | −61.0 (3) | C17—S3—C18—C19 | −52.0 (3) |
Fe1i—S3—C18—C21 | −178.3 (3) | C17—S3—C18—C20 | −171.7 (3) |
Fe1—O1—C27—C22 | 51.3 (6) | C17—S3—C18—C21 | 71.0 (3) |
Fe1—O1—C27—C26 | −129.2 (4) | C18—S3—C17—B1 | −104.9 (3) |
S1—Fe1—O1—C27 | −85.7 (4) | C22—C23—C24—C25 | 1.1 (9) |
S1—C7—B1—C6 | 168.3 (3) | C23—C22—C27—O1 | −179.7 (4) |
S1—C7—B1—C12 | −74.0 (4) | C23—C22—C27—C26 | 0.8 (7) |
S1—C7—B1—C17 | 49.5 (4) | C23—C24—C25—C26 | −1.3 (9) |
S2—Fe1—O1—C27 | 22.4 (5) | C24—C25—C26—C27 | 1.2 (9) |
S2—C12—B1—C6 | −172.5 (2) | C25—C26—C27—O1 | 179.5 (5) |
S2—C12—B1—C7 | 73.0 (3) | C25—C26—C27—C22 | −0.9 (7) |
S2—C12—B1—C17 | −47.8 (4) | C27—C22—C23—C24 | −0.9 (8) |
S3i—Fe1—O1—C27 | 152.9 (4) | C28A—C29A—C30A—C31A | 0.0 |
S3—C17—B1—C6 | 82.4 (3) | C29A—C28A—C33A—C32A | 0.0 |
S3—C17—B1—C7 | −164.0 (2) | C29A—C28A—C33A—C34A | −172.2 (11) |
S3—C17—B1—C12 | −40.9 (4) | C29A—C30A—C31A—C32A | 0.0 |
C1—C2—C3—C4 | −0.5 (7) | C30A—C31A—C32A—C33A | 0.0 |
C1—C6—B1—C7 | −61.6 (4) | C31A—C32A—C33A—C28A | 0.0 |
C1—C6—B1—C12 | 179.1 (3) | C31A—C32A—C33A—C34A | 172.3 (11) |
C1—C6—B1—C17 | 54.3 (5) | C33A—C28A—C29A—C30A | 0.0 |
C2—C1—C6—C5 | 0.5 (6) | C32B—C31B—C30B—C29B | 0.0 |
C2—C1—C6—B1 | 179.7 (4) | C31B—C32B—C33B—C28B | 0.0 |
C2—C3—C4—C5 | −0.8 (8) | C31B—C32B—C33B—C34B | 169 (2) |
C3—C4—C5—C6 | 2.0 (7) | C31B—C30B—C29B—C28B | 0.0 |
C4—C5—C6—C1 | −1.8 (6) | C30B—C29B—C28B—C33B | 0.0 |
C4—C5—C6—B1 | 179.1 (4) | C29B—C28B—C33B—C32B | 0.0 |
C5—C6—B1—C7 | 117.5 (4) | C29B—C28B—C33B—C34B | −169 (2) |
C5—C6—B1—C12 | −1.8 (5) | C33B—C32B—C31B—C30B | 0.0 |
Symmetry code: (i) −x+2, −y, −z+1. |
[Co2(C21H37BO2S3)2] | F(000) = 1036 |
Mr = 974.85 | Dx = 1.263 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 14.409 (4) Å | Cell parameters from 2455 reflections |
b = 9.494 (2) Å | θ = 2.4–21.0° |
c = 18.745 (5) Å | µ = 0.93 mm−1 |
β = 90.938 (4)° | T = 200 K |
V = 2564.0 (11) Å3 | Needle, green |
Z = 2 | 0.14 × 0.09 × 0.08 mm |
Bruker APEXII CCD diffractometer | 5489 independent reflections |
Radiation source: sealed-tube | 3361 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.089 |
Detector resolution: 8.33 pixels mm-1 | θmax = 26.8°, θmin = 1.8° |
φ and ω scans | h = −18→18 |
Absorption correction: multi-scan (APEX2; Bruker, 2007) | k = −12→12 |
Tmin = 0.635, Tmax = 0.745 | l = −23→23 |
28200 measured reflections |
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.047 | H-atom parameters constrained |
wR(F2) = 0.112 | w = 1/[σ2(Fo2) + (0.0441P)2 + 0.6685P] where P = (Fo2 + 2Fc2)/3 |
S = 1.01 | (Δ/σ)max < 0.001 |
5489 reflections | Δρmax = 0.41 e Å−3 |
272 parameters | Δρmin = −0.35 e Å−3 |
35 restraints |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co1 | 1.06446 (3) | 0.52936 (5) | 1.06451 (2) | 0.03513 (14) | |
S2 | 0.85689 (6) | 0.28914 (9) | 0.86910 (4) | 0.0365 (2) | |
S3 | 0.57208 (6) | 0.54967 (10) | 0.88308 (5) | 0.0478 (3) | |
O1 | 0.80143 (15) | 0.5617 (2) | 0.93770 (11) | 0.0358 (5) | |
O2 | 0.94820 (16) | 0.5961 (2) | 1.01995 (11) | 0.0435 (6) | |
C6 | 0.7613 (2) | 0.3999 (4) | 0.83631 (17) | 0.0392 (8) | |
H6A | 0.758820 | 0.393587 | 0.783600 | 0.047* | |
H6B | 0.702401 | 0.360764 | 0.854246 | 0.047* | |
C7 | 0.8054 (3) | 0.1546 (4) | 0.92742 (18) | 0.0443 (9) | |
C8 | 0.8882 (3) | 0.0695 (4) | 0.9543 (2) | 0.0628 (12) | |
H8A | 0.866751 | −0.005417 | 0.986004 | 0.094* | |
H8B | 0.931086 | 0.131440 | 0.980585 | 0.094* | |
H8C | 0.920092 | 0.027700 | 0.913691 | 0.094* | |
C9 | 0.7394 (3) | 0.0625 (4) | 0.8830 (2) | 0.0732 (14) | |
H9A | 0.715000 | −0.013227 | 0.912886 | 0.110* | |
H9B | 0.772966 | 0.021550 | 0.842949 | 0.110* | |
H9C | 0.687820 | 0.120043 | 0.864629 | 0.110* | |
C10 | 0.7552 (3) | 0.2221 (5) | 0.9891 (2) | 0.0649 (12) | |
H10A | 0.730824 | 0.148544 | 1.020298 | 0.097* | |
H10B | 0.703782 | 0.279789 | 0.970585 | 0.097* | |
H10C | 0.798563 | 0.281788 | 1.016290 | 0.097* | |
C11 | 0.6676 (2) | 0.6425 (4) | 0.84372 (18) | 0.0419 (9) | |
H11A | 0.656719 | 0.649077 | 0.791548 | 0.050* | |
H11B | 0.669747 | 0.739570 | 0.862986 | 0.050* | |
C12 | 0.4684 (2) | 0.6589 (4) | 0.8648 (2) | 0.0496 (10) | |
C13 | 0.3900 (3) | 0.5721 (5) | 0.8960 (2) | 0.0684 (13) | |
H13A | 0.330892 | 0.621199 | 0.888099 | 0.103* | |
H13B | 0.401076 | 0.559446 | 0.947298 | 0.103* | |
H13C | 0.387606 | 0.479852 | 0.872588 | 0.103* | |
C14 | 0.4544 (3) | 0.6803 (6) | 0.7859 (2) | 0.0786 (15) | |
H14A | 0.395212 | 0.728595 | 0.776965 | 0.118* | |
H14B | 0.453544 | 0.588613 | 0.761832 | 0.118* | |
H14C | 0.505225 | 0.737496 | 0.767420 | 0.118* | |
C15 | 0.4769 (3) | 0.7994 (5) | 0.9029 (3) | 0.0855 (16) | |
H15A | 0.418728 | 0.851997 | 0.897105 | 0.128* | |
H15B | 0.527831 | 0.853650 | 0.882454 | 0.128* | |
H15C | 0.489599 | 0.783332 | 0.953784 | 0.128* | |
C16 | 0.7138 (2) | 0.7332 (4) | 1.00720 (17) | 0.0401 (8) | |
H16 | 0.659835 | 0.722190 | 0.977950 | 0.048* | |
C17 | 0.7125 (3) | 0.8231 (4) | 1.06582 (18) | 0.0460 (9) | |
H17 | 0.657899 | 0.875201 | 1.075724 | 0.055* | |
C18 | 0.7900 (3) | 0.8372 (4) | 1.10978 (19) | 0.0472 (9) | |
H18 | 0.788262 | 0.897531 | 1.150161 | 0.057* | |
C19 | 0.8698 (3) | 0.7633 (4) | 1.09483 (18) | 0.0456 (9) | |
H19 | 0.923210 | 0.773733 | 1.124732 | 0.055* | |
C20 | 0.8724 (2) | 0.6743 (3) | 1.03658 (16) | 0.0353 (8) | |
C21 | 0.7940 (2) | 0.6599 (3) | 0.99163 (16) | 0.0322 (7) | |
B1 | 0.7668 (3) | 0.5674 (4) | 0.85873 (19) | 0.0345 (9) | |
S1 | 0.95275 (6) | 0.55829 (10) | 0.81592 (5) | 0.0376 (3) | 0.9417 (16) |
C1 | 0.8446 (2) | 0.6582 (4) | 0.81605 (18) | 0.0440 (9) | 0.9417 (16) |
H1A | 0.854621 | 0.750232 | 0.839790 | 0.053* | 0.9417 (16) |
H1B | 0.823044 | 0.675777 | 0.766428 | 0.053* | 0.9417 (16) |
C2 | 1.0490 (3) | 0.6799 (4) | 0.7989 (2) | 0.0514 (10) | 0.9417 (16) |
C3 | 1.0388 (3) | 0.7331 (6) | 0.7226 (2) | 0.0822 (17) | 0.9417 (16) |
H3A | 1.038577 | 0.652933 | 0.689657 | 0.123* | 0.9417 (16) |
H3B | 0.980326 | 0.785143 | 0.717210 | 0.123* | 0.9417 (16) |
H3C | 1.090836 | 0.795538 | 0.711725 | 0.123* | 0.9417 (16) |
C4 | 1.0496 (4) | 0.8009 (5) | 0.8515 (3) | 0.0910 (18) | 0.9417 (16) |
H4A | 1.056191 | 0.763914 | 0.900140 | 0.137* | 0.9417 (16) |
H4B | 1.101703 | 0.863737 | 0.841478 | 0.137* | 0.9417 (16) |
H4C | 0.991193 | 0.853342 | 0.846963 | 0.137* | 0.9417 (16) |
C5 | 1.1365 (3) | 0.5909 (5) | 0.8076 (3) | 0.0862 (17) | 0.9417 (16) |
H5A | 1.134705 | 0.513342 | 0.773168 | 0.129* | 0.9417 (16) |
H5B | 1.191159 | 0.649630 | 0.799196 | 0.129* | 0.9417 (16) |
H5C | 1.139842 | 0.552624 | 0.856161 | 0.129* | 0.9417 (16) |
S1A | 0.9497 (8) | 0.6792 (15) | 0.8660 (6) | 0.0376 (3) | 0.0583 (16) |
C1A | 0.8446 (2) | 0.6582 (4) | 0.81605 (18) | 0.0440 (9) | 0.0583 (16) |
H1AA | 0.818916 | 0.752331 | 0.804487 | 0.053* | 0.0583 (16) |
H1AB | 0.858249 | 0.610181 | 0.770524 | 0.053* | 0.0583 (16) |
C2A | 1.0490 (3) | 0.6799 (4) | 0.7989 (2) | 0.0514 (10) | 0.0583 (16) |
C3A | 1.034 (3) | 0.814 (4) | 0.756 (2) | 0.0822 (17) | 0.0583 (16) |
H3AA | 0.974833 | 0.807073 | 0.729602 | 0.123* | 0.0583 (16) |
H3AB | 1.031909 | 0.894382 | 0.788706 | 0.123* | 0.0583 (16) |
H3AC | 1.084720 | 0.825712 | 0.722801 | 0.123* | 0.0583 (16) |
C4A | 1.032 (3) | 0.549 (4) | 0.754 (2) | 0.0910 (18) | 0.0583 (16) |
H4AA | 0.973122 | 0.559706 | 0.727297 | 0.137* | 0.0583 (16) |
H4AB | 1.082713 | 0.537408 | 0.720497 | 0.137* | 0.0583 (16) |
H4AC | 1.028412 | 0.466654 | 0.785103 | 0.137* | 0.0583 (16) |
C5A | 1.1358 (11) | 0.676 (7) | 0.8417 (16) | 0.0862 (17) | 0.0583 (16) |
H5AA | 1.140038 | 0.586631 | 0.867434 | 0.129* | 0.0583 (16) |
H5AB | 1.188939 | 0.685562 | 0.810038 | 0.129* | 0.0583 (16) |
H5AC | 1.136128 | 0.754232 | 0.875944 | 0.129* | 0.0583 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0380 (3) | 0.0350 (3) | 0.0321 (2) | 0.0048 (2) | −0.0095 (2) | −0.0009 (2) |
S2 | 0.0434 (5) | 0.0338 (5) | 0.0322 (4) | 0.0052 (4) | −0.0046 (4) | −0.0023 (4) |
S3 | 0.0402 (5) | 0.0490 (6) | 0.0538 (6) | −0.0023 (5) | −0.0055 (4) | 0.0057 (5) |
O1 | 0.0399 (13) | 0.0335 (13) | 0.0336 (12) | 0.0043 (10) | −0.0107 (10) | −0.0044 (10) |
O2 | 0.0447 (15) | 0.0465 (15) | 0.0387 (13) | 0.0141 (12) | −0.0161 (11) | −0.0091 (11) |
C6 | 0.041 (2) | 0.041 (2) | 0.0357 (19) | 0.0046 (16) | −0.0119 (16) | 0.0008 (15) |
C7 | 0.056 (2) | 0.037 (2) | 0.039 (2) | −0.0008 (18) | −0.0010 (18) | 0.0019 (16) |
C8 | 0.083 (3) | 0.050 (3) | 0.055 (3) | 0.019 (2) | 0.004 (2) | 0.013 (2) |
C9 | 0.098 (4) | 0.050 (3) | 0.071 (3) | −0.028 (3) | −0.019 (3) | 0.008 (2) |
C10 | 0.070 (3) | 0.069 (3) | 0.057 (3) | 0.004 (2) | 0.020 (2) | 0.009 (2) |
C11 | 0.040 (2) | 0.043 (2) | 0.042 (2) | 0.0016 (17) | −0.0066 (16) | 0.0020 (17) |
C12 | 0.036 (2) | 0.055 (3) | 0.058 (2) | 0.0031 (19) | 0.0011 (19) | −0.003 (2) |
C13 | 0.051 (3) | 0.085 (3) | 0.069 (3) | −0.003 (2) | 0.009 (2) | −0.009 (3) |
C14 | 0.056 (3) | 0.109 (4) | 0.071 (3) | 0.029 (3) | −0.002 (2) | 0.021 (3) |
C15 | 0.061 (3) | 0.067 (3) | 0.129 (4) | 0.013 (3) | 0.006 (3) | −0.019 (3) |
C16 | 0.037 (2) | 0.045 (2) | 0.0390 (19) | −0.0003 (17) | −0.0018 (16) | 0.0016 (16) |
C17 | 0.043 (2) | 0.050 (2) | 0.045 (2) | 0.0063 (18) | 0.0108 (18) | −0.0058 (18) |
C18 | 0.056 (3) | 0.046 (2) | 0.040 (2) | 0.0030 (19) | 0.0022 (19) | −0.0092 (17) |
C19 | 0.049 (2) | 0.048 (2) | 0.039 (2) | 0.0038 (18) | −0.0104 (18) | −0.0093 (17) |
C20 | 0.040 (2) | 0.0347 (19) | 0.0308 (17) | 0.0052 (16) | −0.0031 (15) | 0.0034 (15) |
C21 | 0.037 (2) | 0.0284 (18) | 0.0308 (17) | −0.0001 (15) | −0.0010 (15) | 0.0016 (14) |
B1 | 0.039 (2) | 0.034 (2) | 0.030 (2) | 0.0030 (18) | −0.0092 (17) | −0.0022 (16) |
S1 | 0.0396 (5) | 0.0395 (6) | 0.0337 (5) | 0.0009 (4) | −0.0019 (4) | 0.0005 (4) |
C1 | 0.044 (2) | 0.044 (2) | 0.044 (2) | 0.0052 (17) | −0.0084 (17) | 0.0079 (17) |
C2 | 0.048 (2) | 0.050 (2) | 0.056 (2) | −0.0040 (19) | 0.0086 (19) | 0.0067 (19) |
C3 | 0.079 (4) | 0.098 (4) | 0.069 (3) | −0.027 (3) | 0.008 (3) | 0.035 (3) |
C4 | 0.086 (4) | 0.084 (4) | 0.103 (4) | −0.042 (3) | 0.013 (3) | −0.028 (3) |
C5 | 0.044 (3) | 0.081 (4) | 0.133 (5) | −0.002 (3) | 0.001 (3) | 0.020 (4) |
S1A | 0.0396 (5) | 0.0395 (6) | 0.0337 (5) | 0.0009 (4) | −0.0019 (4) | 0.0005 (4) |
C1A | 0.044 (2) | 0.044 (2) | 0.044 (2) | 0.0052 (17) | −0.0084 (17) | 0.0079 (17) |
C2A | 0.048 (2) | 0.050 (2) | 0.056 (2) | −0.0040 (19) | 0.0086 (19) | 0.0067 (19) |
C3A | 0.079 (4) | 0.098 (4) | 0.069 (3) | −0.027 (3) | 0.008 (3) | 0.035 (3) |
C4A | 0.086 (4) | 0.084 (4) | 0.103 (4) | −0.042 (3) | 0.013 (3) | −0.028 (3) |
C5A | 0.044 (3) | 0.081 (4) | 0.133 (5) | −0.002 (3) | 0.001 (3) | 0.020 (4) |
Co1—S2i | 2.3993 (10) | C16—C17 | 1.392 (5) |
Co1—O1i | 2.118 (2) | C16—C21 | 1.383 (4) |
Co1—O2i | 1.987 (2) | C17—H17 | 0.9500 |
Co1—O2 | 1.965 (2) | C17—C18 | 1.384 (5) |
Co1—S1i | 2.4075 (11) | C18—H18 | 0.9500 |
Co1—S1Ai | 2.381 (14) | C18—C19 | 1.379 (5) |
S2—C6 | 1.831 (3) | C19—H19 | 0.9500 |
S2—C7 | 1.845 (4) | C19—C20 | 1.382 (4) |
S3—C11 | 1.803 (4) | C20—C21 | 1.405 (4) |
S3—C12 | 1.846 (4) | B1—C1 | 1.634 (5) |
O1—C21 | 1.381 (4) | B1—C1A | 1.634 (5) |
O1—B1 | 1.555 (4) | S1—C1 | 1.824 (3) |
O2—C20 | 1.361 (4) | S1—C2 | 1.836 (4) |
C6—H6A | 0.9900 | C1—H1A | 0.9900 |
C6—H6B | 0.9900 | C1—H1B | 0.9900 |
C6—B1 | 1.646 (5) | C2—C3 | 1.523 (5) |
C7—C8 | 1.520 (5) | C2—C4 | 1.513 (6) |
C7—C9 | 1.529 (5) | C2—C5 | 1.524 (5) |
C7—C10 | 1.516 (5) | C3—H3A | 0.9800 |
C8—H8A | 0.9800 | C3—H3B | 0.9800 |
C8—H8B | 0.9800 | C3—H3C | 0.9800 |
C8—H8C | 0.9800 | C4—H4A | 0.9800 |
C9—H9A | 0.9800 | C4—H4B | 0.9800 |
C9—H9B | 0.9800 | C4—H4C | 0.9800 |
C9—H9C | 0.9800 | C5—H5A | 0.9800 |
C10—H10A | 0.9800 | C5—H5B | 0.9800 |
C10—H10B | 0.9800 | C5—H5C | 0.9800 |
C10—H10C | 0.9800 | S1A—C1A | 1.778 (12) |
C11—H11A | 0.9900 | S1A—C2A | 1.920 (12) |
C11—H11B | 0.9900 | C1A—H1AA | 0.9900 |
C11—B1 | 1.618 (5) | C1A—H1AB | 0.9900 |
C12—C13 | 1.522 (5) | C2A—C3A | 1.514 (17) |
C12—C14 | 1.504 (5) | C2A—C4A | 1.517 (17) |
C12—C15 | 1.517 (6) | C2A—C5A | 1.475 (17) |
C13—H13A | 0.9800 | C3A—H3AA | 0.9800 |
C13—H13B | 0.9800 | C3A—H3AB | 0.9800 |
C13—H13C | 0.9800 | C3A—H3AC | 0.9800 |
C14—H14A | 0.9800 | C4A—H4AA | 0.9800 |
C14—H14B | 0.9800 | C4A—H4AB | 0.9800 |
C14—H14C | 0.9800 | C4A—H4AC | 0.9800 |
C15—H15A | 0.9800 | C5A—H5AA | 0.9800 |
C15—H15B | 0.9800 | C5A—H5AB | 0.9800 |
C15—H15C | 0.9800 | C5A—H5AC | 0.9800 |
C16—H16 | 0.9500 | ||
S2i—Co1—S1i | 79.65 (4) | C18—C17—C16 | 120.5 (3) |
O1i—Co1—S2i | 83.10 (6) | C18—C17—H17 | 119.7 |
O1i—Co1—S1i | 89.14 (6) | C17—C18—H18 | 120.1 |
O1i—Co1—S1Ai | 76.0 (3) | C19—C18—C17 | 119.8 (3) |
O2—Co1—S2i | 112.40 (7) | C19—C18—H18 | 120.1 |
O2i—Co1—S2i | 151.66 (8) | C18—C19—H19 | 119.8 |
O2—Co1—O1i | 153.55 (9) | C18—C19—C20 | 120.3 (3) |
O2i—Co1—O1i | 79.15 (8) | C20—C19—H19 | 119.8 |
O2—Co1—O2i | 77.77 (10) | O2—C20—C19 | 123.2 (3) |
O2i—Co1—S1i | 121.67 (8) | O2—C20—C21 | 116.7 (3) |
O2—Co1—S1i | 114.03 (8) | C19—C20—C21 | 120.1 (3) |
O2i—Co1—S1Ai | 86.0 (3) | O1—C21—C16 | 124.7 (3) |
O2—Co1—S1Ai | 114.9 (3) | O1—C21—C20 | 115.7 (3) |
C6—S2—Co1i | 96.20 (11) | C16—C21—C20 | 119.4 (3) |
C6—S2—C7 | 106.78 (17) | O1—B1—C6 | 102.9 (2) |
C7—S2—Co1i | 112.41 (11) | O1—B1—C11 | 116.7 (3) |
C11—S3—C12 | 105.71 (17) | O1—B1—C1 | 105.8 (3) |
C21—O1—Co1i | 111.84 (18) | O1—B1—C1A | 105.8 (3) |
C21—O1—B1 | 130.2 (2) | C11—B1—C6 | 110.0 (3) |
B1—O1—Co1i | 105.92 (18) | C11—B1—C1 | 107.1 (3) |
Co1—O2—Co1i | 102.23 (10) | C11—B1—C1A | 107.1 (3) |
C20—O2—Co1 | 139.5 (2) | C1—B1—C6 | 114.6 (3) |
C20—O2—Co1i | 116.49 (19) | C1A—B1—C6 | 114.6 (3) |
S2—C6—H6A | 108.3 | C1—S1—Co1i | 94.45 (11) |
S2—C6—H6B | 108.3 | C1—S1—C2 | 108.69 (18) |
H6A—C6—H6B | 107.4 | C2—S1—Co1i | 117.94 (13) |
B1—C6—S2 | 115.8 (2) | B1—C1—S1 | 108.6 (2) |
B1—C6—H6A | 108.3 | B1—C1—H1A | 110.0 |
B1—C6—H6B | 108.3 | B1—C1—H1B | 110.0 |
C8—C7—S2 | 104.1 (3) | S1—C1—H1A | 110.0 |
C8—C7—C9 | 110.8 (3) | S1—C1—H1B | 110.0 |
C9—C7—S2 | 109.0 (3) | H1A—C1—H1B | 108.4 |
C10—C7—S2 | 111.1 (3) | C3—C2—S1 | 108.1 (3) |
C10—C7—C8 | 110.7 (3) | C3—C2—C5 | 110.6 (4) |
C10—C7—C9 | 111.0 (3) | C4—C2—S1 | 111.1 (3) |
C7—C8—H8A | 109.5 | C4—C2—C3 | 111.1 (4) |
C7—C8—H8B | 109.5 | C4—C2—C5 | 110.8 (4) |
C7—C8—H8C | 109.5 | C5—C2—S1 | 105.0 (3) |
H8A—C8—H8B | 109.5 | C2—C3—H3A | 109.5 |
H8A—C8—H8C | 109.5 | C2—C3—H3B | 109.5 |
H8B—C8—H8C | 109.5 | C2—C3—H3C | 109.5 |
C7—C9—H9A | 109.5 | H3A—C3—H3B | 109.5 |
C7—C9—H9B | 109.5 | H3A—C3—H3C | 109.5 |
C7—C9—H9C | 109.5 | H3B—C3—H3C | 109.5 |
H9A—C9—H9B | 109.5 | C2—C4—H4A | 109.5 |
H9A—C9—H9C | 109.5 | C2—C4—H4B | 109.5 |
H9B—C9—H9C | 109.5 | C2—C4—H4C | 109.5 |
C7—C10—H10A | 109.5 | H4A—C4—H4B | 109.5 |
C7—C10—H10B | 109.5 | H4A—C4—H4C | 109.5 |
C7—C10—H10C | 109.5 | H4B—C4—H4C | 109.5 |
H10A—C10—H10B | 109.5 | C2—C5—H5A | 109.5 |
H10A—C10—H10C | 109.5 | C2—C5—H5B | 109.5 |
H10B—C10—H10C | 109.5 | C2—C5—H5C | 109.5 |
S3—C11—H11A | 109.0 | H5A—C5—H5B | 109.5 |
S3—C11—H11B | 109.0 | H5A—C5—H5C | 109.5 |
H11A—C11—H11B | 107.8 | H5B—C5—H5C | 109.5 |
B1—C11—S3 | 113.1 (2) | C1A—S1A—C2A | 107.0 (6) |
B1—C11—H11A | 109.0 | B1—C1A—S1A | 112.7 (5) |
B1—C11—H11B | 109.0 | B1—C1A—H1AA | 109.0 |
C13—C12—S3 | 103.2 (3) | B1—C1A—H1AB | 109.0 |
C14—C12—S3 | 110.7 (3) | S1A—C1A—H1AA | 109.0 |
C14—C12—C13 | 111.2 (3) | S1A—C1A—H1AB | 109.0 |
C14—C12—C15 | 110.7 (4) | H1AA—C1A—H1AB | 107.8 |
C15—C12—S3 | 110.3 (3) | C3A—C2A—S1A | 104.2 (11) |
C15—C12—C13 | 110.5 (3) | C3A—C2A—C4A | 111.7 (13) |
C12—C13—H13A | 109.5 | C4A—C2A—S1A | 104.1 (11) |
C12—C13—H13B | 109.5 | C5A—C2A—S1A | 106.2 (12) |
C12—C13—H13C | 109.5 | C5A—C2A—C3A | 114.9 (14) |
H13A—C13—H13B | 109.5 | C5A—C2A—C4A | 114.3 (13) |
H13A—C13—H13C | 109.5 | C2A—C3A—H3AA | 109.5 |
H13B—C13—H13C | 109.5 | C2A—C3A—H3AB | 109.5 |
C12—C14—H14A | 109.5 | C2A—C3A—H3AC | 109.5 |
C12—C14—H14B | 109.5 | H3AA—C3A—H3AB | 109.5 |
C12—C14—H14C | 109.5 | H3AA—C3A—H3AC | 109.5 |
H14A—C14—H14B | 109.5 | H3AB—C3A—H3AC | 109.5 |
H14A—C14—H14C | 109.5 | C2A—C4A—H4AA | 109.5 |
H14B—C14—H14C | 109.5 | C2A—C4A—H4AB | 109.5 |
C12—C15—H15A | 109.5 | C2A—C4A—H4AC | 109.5 |
C12—C15—H15B | 109.5 | H4AA—C4A—H4AB | 109.5 |
C12—C15—H15C | 109.5 | H4AA—C4A—H4AC | 109.5 |
H15A—C15—H15B | 109.5 | H4AB—C4A—H4AC | 109.5 |
H15A—C15—H15C | 109.5 | C2A—C5A—H5AA | 109.5 |
H15B—C15—H15C | 109.5 | C2A—C5A—H5AB | 109.5 |
C17—C16—H16 | 120.1 | C2A—C5A—H5AC | 109.5 |
C21—C16—H16 | 120.1 | H5AA—C5A—H5AB | 109.5 |
C21—C16—C17 | 119.8 (3) | H5AA—C5A—H5AC | 109.5 |
C16—C17—H17 | 119.7 | H5AB—C5A—H5AC | 109.5 |
Co1i—S2—C6—B1 | 2.7 (3) | C6—S2—C7—C9 | 63.3 (3) |
Co1i—S2—C7—C8 | −74.2 (2) | C6—S2—C7—C10 | −59.3 (3) |
Co1i—S2—C7—C9 | 167.6 (2) | C6—B1—C1—S1 | −46.1 (3) |
Co1i—S2—C7—C10 | 45.0 (3) | C6—B1—C1A—S1A | −98.2 (6) |
Co1i—O1—C21—C16 | −178.0 (3) | C7—S2—C6—B1 | 118.4 (3) |
Co1i—O1—C21—C20 | −3.8 (3) | C11—S3—C12—C13 | 177.4 (2) |
Co1i—O1—B1—C6 | 63.4 (3) | C11—S3—C12—C14 | 58.3 (3) |
Co1i—O1—B1—C11 | −176.0 (2) | C11—S3—C12—C15 | −64.5 (3) |
Co1i—O1—B1—C1 | −57.1 (3) | C11—B1—C1—S1 | −168.4 (2) |
Co1i—O1—B1—C1A | −57.1 (3) | C11—B1—C1A—S1A | 139.5 (5) |
Co1—O2—C20—C19 | 16.7 (5) | C12—S3—C11—B1 | 176.2 (2) |
Co1i—O2—C20—C19 | 178.2 (3) | C16—C17—C18—C19 | 1.0 (6) |
Co1—O2—C20—C21 | −162.5 (2) | C17—C16—C21—O1 | 175.8 (3) |
Co1i—O2—C20—C21 | −1.1 (4) | C17—C16—C21—C20 | 1.8 (5) |
Co1i—S1—C1—B1 | −38.0 (2) | C17—C18—C19—C20 | −0.6 (6) |
Co1i—S1—C2—C3 | −173.6 (3) | C18—C19—C20—O2 | −178.4 (3) |
Co1i—S1—C2—C4 | −51.5 (3) | C18—C19—C20—C21 | 0.8 (5) |
Co1i—S1—C2—C5 | 68.4 (3) | C19—C20—C21—O1 | −175.9 (3) |
Co1i—S1A—C1A—B1 | 26.9 (6) | C19—C20—C21—C16 | −1.4 (5) |
S2—C6—B1—O1 | −40.8 (3) | C21—O1—B1—C6 | −158.2 (3) |
S2—C6—B1—C11 | −165.8 (2) | C21—O1—B1—C11 | −37.7 (5) |
S2—C6—B1—C1 | 73.5 (3) | C21—O1—B1—C1 | 81.3 (4) |
S2—C6—B1—C1A | 73.5 (3) | C21—O1—B1—C1A | 81.3 (4) |
S3—C11—B1—O1 | −65.0 (3) | C21—C16—C17—C18 | −1.6 (5) |
S3—C11—B1—C6 | 51.7 (3) | B1—O1—C21—C16 | 45.5 (5) |
S3—C11—B1—C1 | 176.7 (2) | B1—O1—C21—C20 | −140.3 (3) |
S3—C11—B1—C1A | 176.7 (2) | C1—S1—C2—C3 | −67.8 (3) |
O1—B1—C1—S1 | 66.4 (3) | C1—S1—C2—C4 | 54.3 (4) |
O1—B1—C1A—S1A | 14.4 (6) | C1—S1—C2—C5 | 174.1 (3) |
O2—C20—C21—O1 | 3.3 (4) | C2—S1—C1—B1 | −159.4 (2) |
O2—C20—C21—C16 | 177.9 (3) | C2A—S1A—C1A—B1 | 146.3 (5) |
C6—S2—C7—C8 | −178.4 (2) |
Symmetry code: (i) −x+2, −y+1, −z+2. |
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