Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101021370/na1547sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270101021370/na1547Isup2.hkl |
CCDC reference: 182975
Antimony trichloride (0.049 g, 0.22 mmol) in acetonitrile (5 ml) was added to a 50 ml flask containing triphenylphosphinoferrocene (0.121 g, 0.22 mmol) solution (20 ml). The mixture was stirred at ambient temperature for about 30 min. After stirring, the solution was filtered into another flask and left to evaporate. After 4 d, light-yellow crystals of (I) were obtained. The crystal was washed with acetonitrile.
After checking their presence in the difference map, all H atoms were geometrically fixed and allowed to ride on their parent atoms. The highest peak (0.70 e Å-3) and the deepest hole (-1.01 e Å-3) were found near P2 (1.35 Å) and Sb1 (1.09 Å), respectively.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990).
2[Fe(C17H14P)2]·[Sb4Cl16]·C2H6O | F(000) = 2156 |
Mr = 2208.98 | Dx = 1.633 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 11.6280 (3) Å | Cell parameters from 6411 reflections |
b = 15.0898 (3) Å | θ = 1.6–28.4° |
c = 25.6100 (6) Å | µ = 2.08 mm−1 |
β = 90.342 (1)° | T = 293 K |
V = 4493.56 (18) Å3 | Slab, light yellow |
Z = 2 | 0.34 × 0.22 × 0.20 mm |
Siemens SMART CCD area-detector diffractometer | 7901 independent reflections |
Radiation source: fine-focus sealed tube | 5408 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.084 |
Detector resolution: 8.33 pixels mm-1 | θmax = 25°, θmin = 1.6° |
ω scans | h = −13→13 |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | k = −13→17 |
Tmin = 0.538, Tmax = 0.681 | l = −30→30 |
25353 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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 0.96 | w = 1/[σ2(Fo2) + (0.0396P)2] where P = (Fo2 + 2Fc2)/3 |
7901 reflections | (Δ/σ)max = 0.001 |
454 parameters | Δρmax = 0.70 e Å−3 |
0 restraints | Δρmin = −1.01 e Å−3 |
2[Fe(C17H14P)2]·[Sb4Cl16]·C2H6O | V = 4493.56 (18) Å3 |
Mr = 2208.98 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.6280 (3) Å | µ = 2.08 mm−1 |
b = 15.0898 (3) Å | T = 293 K |
c = 25.6100 (6) Å | 0.34 × 0.22 × 0.20 mm |
β = 90.342 (1)° |
Siemens SMART CCD area-detector diffractometer | 7901 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 5408 reflections with I > 2σ(I) |
Tmin = 0.538, Tmax = 0.681 | Rint = 0.084 |
25353 measured reflections |
R[F2 > 2σ(F2)] = 0.042 | 0 restraints |
wR(F2) = 0.108 | H-atom parameters constrained |
S = 0.96 | Δρmax = 0.70 e Å−3 |
7901 reflections | Δρmin = −1.01 e Å−3 |
454 parameters |
Experimental. The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different ϕ angle (0, 88 and 180°) for the crystal and each exposure of 30 s covered 0.3° in ω. The crystal-to-detector distance was 4 cm and the detector swing angle was -35°. Crystal decay was monitored by repeating 30 initial frames at the end of data collection and analysing the intensity of duplicate reflections, and was found to be negligible. |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Due to a large fraction of weak data at higher angles, the 2θ maximum was limited to 50°. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
P1 | 0.06070 (13) | 0.10346 (10) | 0.38437 (6) | 0.0433 (4) | |
P2 | −0.06959 (13) | 0.08754 (11) | 0.11906 (6) | 0.0477 (4) | |
Sb1 | 0.04900 (3) | 0.40707 (2) | 0.436254 (14) | 0.03956 (12) | |
Sb2 | 0.02832 (3) | 0.33168 (3) | 0.609368 (14) | 0.04211 (13) | |
Fe1 | 0.0000 | 0.0000 | 0.5000 | 0.0429 (3) | |
Fe2 | 0.0000 | 0.0000 | 0.0000 | 0.0433 (3) | |
Cl1 | −0.05782 (15) | 0.28880 (11) | 0.48777 (7) | 0.0658 (5) | |
Cl2 | 0.21074 (13) | 0.30805 (11) | 0.42200 (7) | 0.0637 (5) | |
Cl3 | −0.04939 (15) | 0.35352 (12) | 0.35981 (6) | 0.0657 (5) | |
Cl4 | 0.14821 (13) | 0.53149 (12) | 0.37275 (6) | 0.0656 (5) | |
Cl5 | 0.11886 (13) | 0.39306 (12) | 0.68552 (6) | 0.0630 (5) | |
Cl6 | −0.08023 (16) | 0.22344 (12) | 0.66150 (7) | 0.0758 (5) | |
Cl7 | 0.19149 (15) | 0.23228 (12) | 0.59678 (7) | 0.0683 (5) | |
Cl8 | 0.14619 (12) | 0.46402 (11) | 0.54968 (6) | 0.0538 (4) | |
O1 | 0.488 (2) | 0.084 (3) | 0.5520 (10) | 0.33 (2) | 0.50 |
H1A | 0.4572 | 0.1122 | 0.5752 | 0.501* | 0.50 |
C1 | 0.1009 (5) | 0.0437 (4) | 0.4408 (2) | 0.0433 (14) | |
C2 | 0.1152 (5) | −0.0501 (4) | 0.4466 (2) | 0.0508 (15) | |
H2A | 0.0994 | −0.0954 | 0.4201 | 0.061* | |
C3 | 0.1567 (5) | −0.0652 (5) | 0.4986 (2) | 0.0566 (17) | |
H3A | 0.1727 | −0.1233 | 0.5142 | 0.068* | |
C4 | 0.1699 (5) | 0.0175 (5) | 0.5239 (2) | 0.0574 (18) | |
H4A | 0.1960 | 0.0262 | 0.5600 | 0.069* | |
C5 | 0.1363 (5) | 0.0853 (4) | 0.4891 (2) | 0.0476 (15) | |
H5A | 0.1368 | 0.1490 | 0.4964 | 0.057* | |
C6 | 0.1790 (5) | 0.0975 (4) | 0.3400 (2) | 0.0470 (15) | |
C7 | 0.1671 (7) | 0.1248 (7) | 0.2902 (3) | 0.113 (3) | |
H7A | 0.0969 | 0.1471 | 0.2787 | 0.135* | |
C8 | 0.2598 (8) | 0.1198 (8) | 0.2556 (3) | 0.128 (4) | |
H8A | 0.2503 | 0.1370 | 0.2210 | 0.153* | |
C9 | 0.3617 (8) | 0.0902 (6) | 0.2723 (3) | 0.095 (3) | |
H9A | 0.4230 | 0.0852 | 0.2493 | 0.114* | |
C10 | 0.3743 (7) | 0.0681 (7) | 0.3219 (4) | 0.113 (3) | |
H10A | 0.4461 | 0.0491 | 0.3335 | 0.136* | |
C11 | 0.2847 (6) | 0.0721 (6) | 0.3572 (3) | 0.099 (3) | |
H11A | 0.2967 | 0.0577 | 0.3921 | 0.119* | |
C12 | −0.0696 (5) | 0.0660 (4) | 0.3538 (2) | 0.0443 (14) | |
C13 | −0.0766 (6) | −0.0130 (5) | 0.3279 (3) | 0.0666 (19) | |
H13A | −0.0115 | −0.0483 | 0.3244 | 0.080* | |
C14 | −0.1797 (7) | −0.0402 (6) | 0.3072 (3) | 0.085 (2) | |
H14A | −0.1847 | −0.0947 | 0.2904 | 0.102* | |
C15 | −0.2737 (7) | 0.0112 (7) | 0.3110 (3) | 0.094 (3) | |
H15A | −0.3424 | −0.0072 | 0.2957 | 0.113* | |
C16 | −0.2694 (7) | 0.0907 (6) | 0.3371 (4) | 0.091 (3) | |
H16A | −0.3355 | 0.1250 | 0.3402 | 0.110* | |
C17 | −0.1680 (6) | 0.1193 (5) | 0.3587 (3) | 0.0675 (19) | |
H17A | −0.1643 | 0.1732 | 0.3763 | 0.081* | |
C18 | −0.0065 (5) | 0.0947 (4) | 0.0562 (2) | 0.0440 (14) | |
C19 | −0.0711 (5) | 0.1225 (4) | 0.0113 (2) | 0.0478 (15) | |
H19A | −0.1531 | 0.1373 | 0.0103 | 0.057* | |
C20 | 0.0058 (5) | 0.1270 (4) | −0.0303 (2) | 0.0521 (16) | |
H20A | −0.0142 | 0.1435 | −0.0662 | 0.063* | |
C21 | 0.1163 (5) | 0.1011 (4) | −0.0127 (2) | 0.0593 (17) | |
H21A | 0.1854 | 0.0971 | −0.0343 | 0.071* | |
C22 | 0.1103 (5) | 0.0810 (4) | 0.0412 (2) | 0.0527 (16) | |
H22A | 0.1740 | 0.0622 | 0.0639 | 0.063* | |
C23 | −0.0249 (5) | 0.1798 (4) | 0.1589 (2) | 0.0550 (17) | |
C24 | 0.0759 (7) | 0.2271 (5) | 0.1489 (3) | 0.084 (2) | |
H24A | 0.1238 | 0.2106 | 0.1216 | 0.101* | |
C25 | 0.1035 (8) | 0.2993 (6) | 0.1802 (4) | 0.109 (3) | |
H25A | 0.1701 | 0.3317 | 0.1740 | 0.130* | |
C26 | 0.0321 (8) | 0.3224 (5) | 0.2202 (3) | 0.093 (3) | |
H26A | 0.0503 | 0.3715 | 0.2406 | 0.112* | |
C27 | −0.0643 (7) | 0.2756 (6) | 0.2309 (3) | 0.091 (3) | |
H27A | −0.1105 | 0.2915 | 0.2589 | 0.109* | |
C28 | −0.0932 (6) | 0.2052 (5) | 0.2003 (3) | 0.074 (2) | |
H28A | −0.1600 | 0.1736 | 0.2074 | 0.089* | |
C29 | −0.0460 (5) | −0.0154 (4) | 0.1515 (2) | 0.0510 (15) | |
C30 | −0.1380 (6) | −0.0735 (5) | 0.1566 (3) | 0.0641 (18) | |
H30A | −0.2103 | −0.0582 | 0.1437 | 0.077* | |
C31 | −0.1212 (8) | −0.1535 (6) | 0.1807 (3) | 0.086 (2) | |
H31A | −0.1830 | −0.1920 | 0.1847 | 0.103* | |
C32 | −0.0157 (9) | −0.1776 (6) | 0.1990 (3) | 0.101 (3) | |
H32A | −0.0067 | −0.2318 | 0.2157 | 0.121* | |
C33 | 0.0777 (8) | −0.1229 (7) | 0.1930 (3) | 0.098 (3) | |
H33A | 0.1504 | −0.1409 | 0.2039 | 0.118* | |
C34 | 0.0612 (6) | −0.0398 (6) | 0.1703 (3) | 0.077 (2) | |
H34A | 0.1226 | −0.0006 | 0.1678 | 0.092* | |
C35 | 0.481 (3) | 0.128 (2) | 0.5074 (18) | 0.19 (2) | 0.50 |
H35A | 0.3998 | 0.1388 | 0.5017 | 0.229* | 0.50 |
H35B | 0.5155 | 0.1855 | 0.5143 | 0.229* | 0.50 |
C36 | 0.521 (3) | 0.103 (2) | 0.4628 (15) | 0.19 (2) | 0.50 |
H36A | 0.5044 | 0.1472 | 0.4369 | 0.292* | 0.50 |
H36B | 0.4859 | 0.0479 | 0.4529 | 0.292* | 0.50 |
H36C | 0.6029 | 0.0951 | 0.4656 | 0.292* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.0466 (9) | 0.0498 (10) | 0.0336 (8) | 0.0002 (7) | 0.0089 (7) | 0.0020 (7) |
P2 | 0.0415 (9) | 0.0678 (11) | 0.0337 (8) | 0.0019 (8) | 0.0019 (7) | −0.0050 (8) |
Sb1 | 0.0406 (2) | 0.0447 (2) | 0.0333 (2) | −0.00056 (18) | −0.00072 (16) | −0.00502 (17) |
Sb2 | 0.0403 (2) | 0.0517 (3) | 0.0345 (2) | −0.00163 (18) | 0.00603 (16) | −0.00355 (18) |
Fe1 | 0.0445 (7) | 0.0510 (8) | 0.0334 (6) | −0.0060 (6) | 0.0065 (5) | 0.0054 (5) |
Fe2 | 0.0390 (6) | 0.0578 (8) | 0.0331 (6) | 0.0086 (6) | 0.0053 (5) | 0.0009 (6) |
Cl1 | 0.0723 (11) | 0.0626 (11) | 0.0626 (11) | −0.0154 (9) | 0.0058 (9) | −0.0009 (9) |
Cl2 | 0.0468 (9) | 0.0665 (11) | 0.0779 (12) | 0.0106 (8) | −0.0023 (8) | −0.0146 (9) |
Cl3 | 0.0755 (11) | 0.0753 (12) | 0.0460 (9) | 0.0001 (9) | −0.0168 (8) | −0.0185 (9) |
Cl4 | 0.0442 (9) | 0.0954 (13) | 0.0572 (10) | 0.0025 (9) | 0.0083 (7) | 0.0109 (10) |
Cl5 | 0.0479 (9) | 0.0969 (14) | 0.0441 (9) | 0.0030 (9) | −0.0002 (7) | −0.0206 (9) |
Cl6 | 0.0838 (13) | 0.0635 (12) | 0.0807 (13) | −0.0065 (10) | 0.0377 (10) | 0.0081 (10) |
Cl7 | 0.0671 (11) | 0.0705 (12) | 0.0675 (11) | 0.0190 (9) | 0.0095 (9) | −0.0139 (9) |
Cl8 | 0.0422 (8) | 0.0681 (11) | 0.0512 (9) | −0.0063 (7) | 0.0051 (7) | −0.0026 (8) |
O1 | 0.158 (18) | 0.62 (6) | 0.22 (3) | 0.02 (3) | −0.01 (2) | −0.28 (3) |
C1 | 0.043 (3) | 0.051 (4) | 0.036 (3) | −0.006 (3) | 0.012 (3) | 0.004 (3) |
C2 | 0.055 (4) | 0.047 (4) | 0.051 (4) | −0.001 (3) | 0.013 (3) | 0.001 (3) |
C3 | 0.047 (4) | 0.064 (5) | 0.059 (4) | 0.005 (3) | 0.009 (3) | 0.021 (4) |
C4 | 0.044 (4) | 0.082 (5) | 0.046 (4) | −0.015 (3) | −0.003 (3) | 0.014 (4) |
C5 | 0.048 (4) | 0.053 (4) | 0.041 (3) | −0.013 (3) | 0.005 (3) | 0.003 (3) |
C6 | 0.051 (4) | 0.062 (4) | 0.029 (3) | −0.001 (3) | 0.011 (3) | 0.005 (3) |
C7 | 0.060 (5) | 0.224 (11) | 0.054 (5) | 0.007 (6) | 0.013 (4) | 0.043 (6) |
C8 | 0.092 (7) | 0.245 (12) | 0.046 (5) | −0.031 (8) | 0.031 (5) | 0.039 (6) |
C9 | 0.086 (6) | 0.135 (8) | 0.064 (5) | −0.006 (6) | 0.043 (5) | 0.004 (5) |
C10 | 0.063 (5) | 0.169 (10) | 0.107 (7) | 0.035 (6) | 0.030 (5) | 0.039 (7) |
C11 | 0.056 (5) | 0.177 (9) | 0.067 (5) | 0.027 (5) | 0.026 (4) | 0.045 (5) |
C12 | 0.045 (3) | 0.054 (4) | 0.034 (3) | −0.001 (3) | 0.003 (3) | 0.011 (3) |
C13 | 0.072 (5) | 0.065 (5) | 0.063 (4) | 0.008 (4) | −0.005 (4) | −0.008 (4) |
C14 | 0.092 (6) | 0.087 (6) | 0.076 (5) | −0.016 (5) | −0.025 (5) | −0.015 (5) |
C15 | 0.072 (6) | 0.120 (8) | 0.090 (6) | −0.023 (6) | −0.028 (5) | 0.018 (6) |
C16 | 0.060 (5) | 0.086 (6) | 0.129 (8) | 0.000 (5) | −0.016 (5) | 0.018 (6) |
C17 | 0.058 (4) | 0.057 (4) | 0.088 (5) | 0.001 (4) | 0.000 (4) | 0.004 (4) |
C18 | 0.043 (3) | 0.055 (4) | 0.034 (3) | 0.007 (3) | 0.003 (3) | −0.001 (3) |
C19 | 0.043 (3) | 0.059 (4) | 0.041 (3) | 0.015 (3) | 0.003 (3) | −0.002 (3) |
C20 | 0.059 (4) | 0.056 (4) | 0.042 (3) | 0.011 (3) | 0.011 (3) | 0.009 (3) |
C21 | 0.055 (4) | 0.060 (4) | 0.063 (4) | 0.001 (3) | 0.024 (3) | −0.008 (3) |
C22 | 0.042 (3) | 0.067 (4) | 0.050 (4) | 0.006 (3) | −0.001 (3) | −0.002 (3) |
C23 | 0.050 (4) | 0.078 (5) | 0.037 (3) | 0.006 (3) | −0.003 (3) | −0.010 (3) |
C24 | 0.080 (6) | 0.100 (6) | 0.073 (5) | −0.028 (5) | 0.025 (4) | −0.018 (5) |
C25 | 0.107 (7) | 0.123 (8) | 0.096 (7) | −0.056 (6) | 0.025 (5) | −0.044 (6) |
C26 | 0.108 (7) | 0.090 (6) | 0.081 (6) | −0.004 (5) | −0.003 (5) | −0.042 (5) |
C27 | 0.063 (5) | 0.140 (8) | 0.070 (5) | −0.010 (5) | 0.003 (4) | −0.048 (5) |
C28 | 0.052 (4) | 0.117 (6) | 0.054 (4) | −0.009 (4) | 0.005 (3) | −0.033 (4) |
C29 | 0.048 (4) | 0.070 (4) | 0.035 (3) | 0.000 (3) | 0.006 (3) | 0.002 (3) |
C30 | 0.061 (4) | 0.073 (5) | 0.058 (4) | 0.000 (4) | 0.003 (3) | 0.000 (4) |
C31 | 0.093 (6) | 0.085 (6) | 0.081 (6) | −0.007 (5) | 0.015 (5) | 0.007 (5) |
C32 | 0.125 (8) | 0.087 (7) | 0.090 (7) | 0.020 (6) | 0.010 (6) | 0.021 (5) |
C33 | 0.084 (6) | 0.119 (8) | 0.090 (6) | 0.033 (6) | −0.009 (5) | 0.030 (6) |
C34 | 0.054 (4) | 0.110 (7) | 0.068 (5) | 0.006 (4) | −0.006 (4) | 0.024 (5) |
C35 | 0.17 (4) | 0.085 (18) | 0.31 (7) | −0.06 (2) | −0.05 (4) | 0.06 (3) |
C36 | 0.11 (2) | 0.19 (4) | 0.28 (5) | 0.015 (19) | −0.04 (3) | 0.12 (4) |
P1—C1 | 1.764 (6) | C11—H11A | 0.9300 |
P1—C6 | 1.792 (6) | C12—C13 | 1.366 (8) |
P1—C12 | 1.793 (6) | C12—C17 | 1.404 (8) |
P2—C18 | 1.776 (6) | C13—C14 | 1.372 (9) |
P2—C29 | 1.782 (6) | C13—H13A | 0.9300 |
P2—C23 | 1.800 (6) | C14—C15 | 1.344 (11) |
Sb1—Cl3 | 2.402 (2) | C14—H14A | 0.9300 |
Sb1—Cl2 | 2.431 (2) | C15—C16 | 1.374 (11) |
Sb1—Cl1 | 2.547 (2) | C15—H15A | 0.9300 |
Sb1—Cl4 | 2.743 (2) | C16—C17 | 1.370 (9) |
Sb1—Cl8i | 3.012 (2) | C16—H16A | 0.9300 |
Sb1—Cl8 | 3.227 (2) | C17—H17A | 0.9300 |
Sb2—Cl5 | 2.397 (2) | C18—C22 | 1.428 (8) |
Sb2—Cl7 | 2.442 (2) | C18—C19 | 1.432 (7) |
Sb2—Cl6 | 2.462 (2) | C19—C20 | 1.397 (8) |
Sb2—Cl8 | 2.869 (2) | C19—H19A | 0.9800 |
Sb2—Cl4i | 2.949 (2) | C20—C21 | 1.414 (8) |
Sb2—Cl1 | 3.329 (2) | C20—H20A | 0.9800 |
Fe1—C1 | 2.032 (5) | C21—C22 | 1.417 (8) |
Fe1—C5 | 2.062 (5) | C21—H21A | 0.9800 |
Fe1—C2 | 2.063 (6) | C22—H22A | 0.9800 |
Fe1—C3 | 2.072 (6) | C23—C28 | 1.384 (8) |
Fe1—C4 | 2.082 (6) | C23—C24 | 1.398 (9) |
Fe2—C18 | 2.030 (5) | C24—C25 | 1.389 (10) |
Fe2—C19 | 2.047 (6) | C24—H24A | 0.9300 |
Fe2—C22 | 2.059 (6) | C25—C26 | 1.369 (11) |
Fe2—C21 | 2.066 (6) | C25—H25A | 0.9300 |
Fe2—C20 | 2.069 (6) | C26—C27 | 1.355 (10) |
O1—C35 | 1.33 (4) | C26—H26A | 0.9300 |
O1—H1A | 0.8200 | C27—C28 | 1.361 (9) |
C1—C2 | 1.433 (8) | C27—H27A | 0.9300 |
C1—C5 | 1.445 (7) | C28—H28A | 0.9300 |
C2—C3 | 1.431 (8) | C29—C34 | 1.384 (8) |
C2—H2A | 0.9800 | C29—C30 | 1.390 (8) |
C3—C4 | 1.415 (8) | C30—C31 | 1.370 (9) |
C3—H3A | 0.9800 | C30—H30A | 0.9300 |
C4—C5 | 1.410 (8) | C31—C32 | 1.359 (11) |
C4—H4A | 0.9800 | C31—H31A | 0.9300 |
C5—H5A | 0.9800 | C32—C33 | 1.373 (11) |
C6—C7 | 1.345 (9) | C32—H32A | 0.9300 |
C6—C11 | 1.358 (8) | C33—C34 | 1.395 (10) |
C7—C8 | 1.402 (10) | C33—H33A | 0.9300 |
C7—H7A | 0.9300 | C34—H34A | 0.9300 |
C8—C9 | 1.334 (11) | C35—C36 | 1.29 (5) |
C8—H8A | 0.9300 | C35—H35A | 0.9700 |
C9—C10 | 1.321 (11) | C35—H35B | 0.9700 |
C9—H9A | 0.9300 | C36—H36A | 0.9600 |
C10—C11 | 1.386 (10) | C36—H36B | 0.9600 |
C10—H10A | 0.9300 | C36—H36C | 0.9600 |
C1—P1—C6 | 107.1 (3) | C6—C7—H7A | 119.7 |
C1—P1—C12 | 114.6 (3) | C8—C7—H7A | 119.7 |
C6—P1—C12 | 110.9 (3) | C9—C8—C7 | 120.0 (8) |
C18—P2—C29 | 114.3 (3) | C9—C8—H8A | 120.0 |
C18—P2—C23 | 110.3 (3) | C7—C8—H8A | 120.0 |
C29—P2—C23 | 111.5 (3) | C10—C9—C8 | 119.1 (8) |
Cl3—Sb1—Cl2 | 92.06 (6) | C10—C9—H9A | 120.5 |
Cl3—Sb1—Cl1 | 87.42 (6) | C8—C9—H9A | 120.5 |
Cl2—Sb1—Cl1 | 91.56 (6) | C9—C10—C11 | 122.5 (8) |
Cl3—Sb1—Cl4 | 86.96 (6) | C9—C10—H10A | 118.8 |
Cl2—Sb1—Cl4 | 90.18 (6) | C11—C10—H10A | 118.8 |
Cl1—Sb1—Cl4 | 174.18 (5) | C6—C11—C10 | 118.9 (7) |
Cl3—Sb1—Cl8i | 87.66 (5) | C6—C11—H11A | 120.6 |
Cl2—Sb1—Cl8i | 177.24 (6) | C10—C11—H11A | 120.6 |
Cl1—Sb1—Cl8i | 91.17 (5) | C13—C12—C17 | 119.8 (6) |
Cl4—Sb1—Cl8i | 87.06 (5) | C13—C12—P1 | 122.3 (5) |
Cl3—Sb1—Cl8 | 170.37 (5) | C17—C12—P1 | 117.9 (5) |
Cl2—Sb1—Cl8 | 91.82 (5) | C12—C13—C14 | 119.8 (7) |
Cl1—Sb1—Cl8 | 83.66 (5) | C12—C13—H13A | 120.1 |
Cl4—Sb1—Cl8 | 101.84 (5) | C14—C13—H13A | 120.1 |
Cl5—Sb2—Cl7 | 90.40 (6) | C15—C14—C13 | 120.6 (8) |
Cl5—Sb2—Cl6 | 92.25 (6) | C15—C14—H14A | 119.7 |
Cl7—Sb2—Cl6 | 93.75 (6) | C13—C14—H14A | 119.7 |
Cl5—Sb2—Cl8 | 87.46 (5) | C14—C15—C16 | 120.8 (7) |
Cl7—Sb2—Cl8 | 89.03 (6) | C14—C15—H15A | 119.6 |
Cl6—Sb2—Cl8 | 177.21 (5) | C16—C15—H15A | 119.6 |
Cl5—Sb2—Cl4i | 84.60 (5) | C17—C16—C15 | 120.0 (8) |
Cl7—Sb2—Cl4i | 173.11 (6) | C17—C16—H16A | 120.0 |
Cl6—Sb2—Cl4i | 91.19 (6) | C15—C16—H16A | 120.0 |
Cl8—Sb2—Cl4i | 86.02 (5) | C16—C17—C12 | 118.9 (7) |
Cl5—Sb2—Cl1 | 164.68 (5) | C16—C17—H17A | 120.6 |
Cl7—Sb2—Cl1 | 89.24 (5) | C12—C17—H17A | 120.6 |
Cl6—Sb2—Cl1 | 103.06 (6) | C22—C18—C19 | 108.8 (5) |
Cl8—Sb2—Cl1 | 77.22 (4) | C22—C18—P2 | 129.3 (4) |
Cl4i—Sb2—Cl1 | 94.33 (5) | C19—C18—P2 | 121.8 (4) |
C1—Fe1—C5 | 41.3 (2) | C22—C18—Fe2 | 70.6 (3) |
C1—Fe1—C5ii | 138.7 (2) | C19—C18—Fe2 | 70.1 (3) |
C1—Fe1—C2 | 41.0 (2) | P2—C18—Fe2 | 128.1 (3) |
C5—Fe1—C2 | 68.7 (2) | C20—C19—C18 | 107.0 (5) |
C5ii—Fe1—C2 | 111.3 (2) | C20—C19—Fe2 | 71.0 (3) |
C1—Fe1—C2ii | 139.0 (2) | C18—C19—Fe2 | 68.8 (3) |
C1ii—Fe1—C3 | 111.7 (2) | C20—C19—H19A | 126.5 |
C1—Fe1—C3 | 68.3 (2) | C18—C19—H19A | 126.5 |
C5—Fe1—C3 | 67.5 (2) | Fe2—C19—H19A | 126.5 |
C2—Fe1—C3 | 40.5 (2) | C19—C20—C21 | 109.1 (5) |
C5—Fe1—C3ii | 112.5 (2) | C19—C20—Fe2 | 69.3 (3) |
C2—Fe1—C3ii | 139.5 (2) | C21—C20—Fe2 | 69.9 (3) |
C1—Fe1—C4 | 68.1 (2) | C19—C20—H20A | 125.4 |
C5—Fe1—C4 | 39.8 (2) | C21—C20—H20A | 125.4 |
C2—Fe1—C4 | 67.8 (2) | Fe2—C20—H20A | 125.4 |
C3—Fe1—C4 | 39.8 (2) | C20—C21—C22 | 108.7 (5) |
C1—Fe1—C4ii | 111.9 (2) | C20—C21—Fe2 | 70.1 (4) |
C5—Fe1—C4ii | 140.2 (2) | C22—C21—Fe2 | 69.6 (4) |
C2—Fe1—C4ii | 112.2 (2) | C20—C21—H21A | 125.7 |
C3—Fe1—C4ii | 140.2 (2) | C22—C21—H21A | 125.7 |
C18—Fe2—C19iii | 138.9 (2) | Fe2—C21—H21A | 125.7 |
C18—Fe2—C19 | 41.1 (2) | C21—C22—C18 | 106.4 (5) |
C18—Fe2—C22iii | 139.1 (2) | C21—C22—Fe2 | 70.2 (3) |
C19—Fe2—C22iii | 111.0 (2) | C18—C22—Fe2 | 68.5 (3) |
C18—Fe2—C22 | 40.9 (2) | C21—C22—H22A | 126.8 |
C19—Fe2—C22 | 69.0 (2) | C18—C22—H22A | 126.8 |
C18—Fe2—C21iii | 112.4 (2) | Fe2—C22—H22A | 126.8 |
C19—Fe2—C21iii | 112.3 (2) | C28—C23—C24 | 119.0 (6) |
C22—Fe2—C21iii | 139.8 (2) | C28—C23—P2 | 118.9 (5) |
C18—Fe2—C21 | 67.6 (2) | C24—C23—P2 | 122.1 (5) |
C19—Fe2—C21 | 67.7 (2) | C25—C24—C23 | 119.1 (7) |
C22—Fe2—C21 | 40.2 (2) | C25—C24—H24A | 120.4 |
C18—Fe2—C20iii | 112.6 (2) | C23—C24—H24A | 120.4 |
C19—Fe2—C20iii | 140.3 (2) | C26—C25—C24 | 119.6 (8) |
C22—Fe2—C20iii | 112.3 (2) | C26—C25—H25A | 120.2 |
C21—Fe2—C20iii | 140.0 (2) | C24—C25—H25A | 120.2 |
C18—Fe2—C20 | 67.4 (2) | C27—C26—C25 | 121.7 (8) |
C19—Fe2—C20 | 39.7 (2) | C27—C26—H26A | 119.2 |
C22—Fe2—C20 | 67.7 (2) | C25—C26—H26A | 119.2 |
C21—Fe2—C20 | 40.0 (2) | C26—C27—C28 | 119.5 (7) |
C35—O1—H1A | 109.5 | C26—C27—H27A | 120.2 |
C2—C1—C5 | 107.9 (5) | C28—C27—H27A | 120.2 |
C2—C1—P1 | 128.3 (4) | C27—C28—C23 | 121.1 (7) |
C5—C1—P1 | 123.5 (4) | C27—C28—H28A | 119.4 |
C2—C1—Fe1 | 70.7 (3) | C23—C28—H28A | 119.4 |
C5—C1—Fe1 | 70.4 (3) | C34—C29—C30 | 119.4 (6) |
P1—C1—Fe1 | 128.7 (3) | C34—C29—P2 | 122.1 (5) |
C3—C2—C1 | 107.0 (5) | C30—C29—P2 | 118.5 (5) |
C3—C2—Fe1 | 70.1 (3) | C31—C30—C29 | 119.4 (7) |
C1—C2—Fe1 | 68.3 (3) | C31—C30—H30A | 120.3 |
C3—C2—H2A | 126.5 | C29—C30—H30A | 120.3 |
C1—C2—H2A | 126.5 | C32—C31—C30 | 121.1 (8) |
Fe1—C2—H2A | 126.5 | C32—C31—H31A | 119.4 |
C4—C3—C2 | 108.7 (6) | C30—C31—H31A | 119.4 |
C4—C3—Fe1 | 70.5 (4) | C31—C32—C33 | 120.9 (8) |
C2—C3—Fe1 | 69.4 (3) | C31—C32—H32A | 119.5 |
C4—C3—H3A | 125.7 | C33—C32—H32A | 119.5 |
C2—C3—H3A | 125.7 | C32—C33—C34 | 118.6 (8) |
Fe1—C3—H3A | 125.7 | C32—C33—H33A | 120.7 |
C5—C4—C3 | 108.8 (5) | C34—C33—H33A | 120.7 |
C5—C4—Fe1 | 69.3 (3) | C29—C34—C33 | 120.4 (7) |
C3—C4—Fe1 | 69.7 (3) | C29—C34—H34A | 119.8 |
C5—C4—H4A | 125.6 | C33—C34—H34A | 119.8 |
C3—C4—H4A | 125.6 | C36—C35—O1 | 126 (4) |
Fe1—C4—H4A | 125.6 | C36—C35—H35A | 105.8 |
C4—C5—C1 | 107.6 (5) | O1—C35—H35A | 105.8 |
C4—C5—Fe1 | 70.9 (3) | C36—C35—H35B | 105.8 |
C1—C5—Fe1 | 68.2 (3) | O1—C35—H35B | 105.8 |
C4—C5—H5A | 126.2 | H35A—C35—H35B | 106.2 |
C1—C5—H5A | 126.2 | C35—C36—H36A | 109.5 |
Fe1—C5—H5A | 126.2 | C35—C36—H36B | 109.5 |
C7—C6—C11 | 118.8 (6) | H36A—C36—H36B | 109.5 |
C7—C6—P1 | 120.7 (5) | C35—C36—H36C | 109.5 |
C11—C6—P1 | 120.3 (5) | H36A—C36—H36C | 109.5 |
C6—C7—C8 | 120.5 (7) | H36B—C36—H36C | 109.5 |
C6—P1—C1—C2 | −70.1 (6) | C29—P2—C18—C22 | −54.8 (6) |
C12—P1—C1—C2 | 53.4 (6) | C23—P2—C18—C22 | 71.8 (6) |
C6—P1—C1—C5 | 103.6 (5) | C29—P2—C18—C19 | 129.3 (5) |
C12—P1—C1—C5 | −133.0 (5) | C23—P2—C18—C19 | −104.1 (5) |
C6—P1—C1—Fe1 | −165.5 (4) | C29—P2—C18—Fe2 | 40.7 (4) |
C12—P1—C1—Fe1 | −42.0 (5) | C23—P2—C18—Fe2 | 167.3 (3) |
C5—Fe1—C1—C2 | 118.1 (5) | C19iii—Fe2—C18—C22 | 60.6 (5) |
C5ii—Fe1—C1—C2 | −61.9 (5) | C19—Fe2—C18—C22 | −119.4 (5) |
C2ii—Fe1—C1—C2 | 180.000 (1) | C22iii—Fe2—C18—C22 | 180.0 |
C3—Fe1—C1—C2 | 37.9 (4) | C21iii—Fe2—C18—C22 | 141.9 (3) |
C3ii—Fe1—C1—C2 | −142.1 (4) | C21—Fe2—C18—C22 | −38.2 (3) |
C4—Fe1—C1—C2 | 80.9 (4) | C20iii—Fe2—C18—C22 | 98.4 (4) |
C4ii—Fe1—C1—C2 | −99.1 (4) | C20—Fe2—C18—C22 | −81.6 (4) |
C5ii—Fe1—C1—C5 | 180.0 | C19iii—Fe2—C18—C19 | 180.0 |
C2—Fe1—C1—C5 | −118.1 (5) | C22iii—Fe2—C18—C19 | −60.6 (5) |
C2ii—Fe1—C1—C5 | 61.9 (5) | C22—Fe2—C18—C19 | 119.4 (5) |
C3—Fe1—C1—C5 | −80.2 (4) | C21iii—Fe2—C18—C19 | −98.8 (4) |
C3ii—Fe1—C1—C5 | 99.8 (4) | C21—Fe2—C18—C19 | 81.2 (4) |
C4—Fe1—C1—C5 | −37.2 (3) | C20iii—Fe2—C18—C19 | −142.2 (3) |
C4ii—Fe1—C1—C5 | 142.8 (3) | C20—Fe2—C18—C19 | 37.8 (3) |
C5—Fe1—C1—P1 | −117.8 (6) | C19iii—Fe2—C18—P2 | −64.6 (5) |
C5ii—Fe1—C1—P1 | 62.2 (6) | C19—Fe2—C18—P2 | 115.4 (5) |
C2—Fe1—C1—P1 | 124.1 (6) | C22iii—Fe2—C18—P2 | 54.8 (5) |
C2ii—Fe1—C1—P1 | −55.9 (6) | C22—Fe2—C18—P2 | −125.2 (5) |
C3—Fe1—C1—P1 | 162.0 (5) | C21iii—Fe2—C18—P2 | 16.6 (4) |
C3ii—Fe1—C1—P1 | −18.0 (5) | C21—Fe2—C18—P2 | −163.4 (4) |
C4—Fe1—C1—P1 | −154.9 (5) | C20iii—Fe2—C18—P2 | −26.8 (4) |
C4ii—Fe1—C1—P1 | 25.1 (5) | C20—Fe2—C18—P2 | 153.2 (4) |
C5—C1—C2—C3 | 1.2 (6) | C22—C18—C19—C20 | −0.9 (7) |
P1—C1—C2—C3 | 175.7 (4) | P2—C18—C19—C20 | 175.7 (4) |
Fe1—C1—C2—C3 | −59.7 (4) | Fe2—C18—C19—C20 | −61.1 (4) |
C5—C1—C2—Fe1 | 60.9 (4) | C22—C18—C19—Fe2 | 60.2 (4) |
P1—C1—C2—Fe1 | −124.6 (5) | P2—C18—C19—Fe2 | −123.2 (4) |
C1ii—Fe1—C2—C3 | −61.4 (5) | C18iii—Fe2—C19—C20 | −62.3 (5) |
C1—Fe1—C2—C3 | 118.6 (5) | C18—Fe2—C19—C20 | 117.7 (5) |
C5—Fe1—C2—C3 | 79.9 (4) | C22iii—Fe2—C19—C20 | −100.0 (4) |
C5ii—Fe1—C2—C3 | −100.1 (4) | C22—Fe2—C19—C20 | 80.0 (4) |
C3ii—Fe1—C2—C3 | 180.000 (2) | C21iii—Fe2—C19—C20 | −143.4 (4) |
C4—Fe1—C2—C3 | 36.9 (4) | C21—Fe2—C19—C20 | 36.6 (4) |
C4ii—Fe1—C2—C3 | −143.1 (4) | C20iii—Fe2—C19—C20 | 180.0 |
C1ii—Fe1—C2—C1 | 180.000 (1) | C18iii—Fe2—C19—C18 | 180.0 |
C5—Fe1—C2—C1 | −38.7 (3) | C22iii—Fe2—C19—C18 | 142.4 (3) |
C5ii—Fe1—C2—C1 | 141.3 (3) | C22—Fe2—C19—C18 | −37.6 (3) |
C3—Fe1—C2—C1 | −118.6 (5) | C21iii—Fe2—C19—C18 | 99.0 (4) |
C3ii—Fe1—C2—C1 | 61.4 (5) | C21—Fe2—C19—C18 | −81.0 (4) |
C4—Fe1—C2—C1 | −81.7 (4) | C20iii—Fe2—C19—C18 | 62.3 (5) |
C4ii—Fe1—C2—C1 | 98.3 (4) | C20—Fe2—C19—C18 | −117.7 (5) |
C1—C2—C3—C4 | −1.2 (6) | C18—C19—C20—C21 | 1.1 (7) |
Fe1—C2—C3—C4 | −59.8 (4) | Fe2—C19—C20—C21 | −58.6 (4) |
C1—C2—C3—Fe1 | 58.6 (4) | C18—C19—C20—Fe2 | 59.7 (4) |
C1ii—Fe1—C3—C4 | −98.6 (4) | C18iii—Fe2—C20—C19 | 140.9 (3) |
C1—Fe1—C3—C4 | 81.4 (4) | C18—Fe2—C20—C19 | −39.1 (3) |
C5—Fe1—C3—C4 | 36.7 (3) | C19iii—Fe2—C20—C19 | 180.0 |
C5ii—Fe1—C3—C4 | −143.3 (3) | C22iii—Fe2—C20—C19 | 96.5 (4) |
C2—Fe1—C3—C4 | 119.7 (5) | C22—Fe2—C20—C19 | −83.5 (4) |
C2ii—Fe1—C3—C4 | −60.3 (5) | C21iii—Fe2—C20—C19 | 59.2 (5) |
C4ii—Fe1—C3—C4 | 180.000 (1) | C21—Fe2—C20—C19 | −120.8 (5) |
C1ii—Fe1—C3—C2 | 141.7 (3) | C18iii—Fe2—C20—C21 | −98.4 (4) |
C1—Fe1—C3—C2 | −38.3 (3) | C18—Fe2—C20—C21 | 81.6 (4) |
C5—Fe1—C3—C2 | −83.1 (4) | C19iii—Fe2—C20—C21 | −59.2 (5) |
C5ii—Fe1—C3—C2 | 96.9 (4) | C19—Fe2—C20—C21 | 120.8 (5) |
C2ii—Fe1—C3—C2 | 180.000 (2) | C22iii—Fe2—C20—C21 | −142.8 (4) |
C4—Fe1—C3—C2 | −119.7 (5) | C22—Fe2—C20—C21 | 37.2 (4) |
C4ii—Fe1—C3—C2 | 60.3 (5) | C21iii—Fe2—C20—C21 | 180.0 |
C2—C3—C4—C5 | 0.7 (7) | C19—C20—C21—C22 | −0.9 (7) |
Fe1—C3—C4—C5 | −58.4 (4) | Fe2—C20—C21—C22 | −59.2 (4) |
C2—C3—C4—Fe1 | 59.1 (4) | C19—C20—C21—Fe2 | 58.3 (4) |
C1ii—Fe1—C4—C5 | −141.5 (3) | C18iii—Fe2—C21—C20 | 99.0 (4) |
C1—Fe1—C4—C5 | 38.5 (3) | C18—Fe2—C21—C20 | −81.0 (4) |
C5ii—Fe1—C4—C5 | 180.0 | C19iii—Fe2—C21—C20 | 143.6 (3) |
C2—Fe1—C4—C5 | 82.9 (4) | C19—Fe2—C21—C20 | −36.4 (3) |
C2ii—Fe1—C4—C5 | −97.1 (4) | C22iii—Fe2—C21—C20 | 60.2 (5) |
C3—Fe1—C4—C5 | 120.4 (5) | C22—Fe2—C21—C20 | −119.8 (5) |
C3ii—Fe1—C4—C5 | −59.6 (5) | C20iii—Fe2—C21—C20 | 180.0 |
C1ii—Fe1—C4—C3 | 98.1 (4) | C18iii—Fe2—C21—C22 | −141.2 (3) |
C1—Fe1—C4—C3 | −81.9 (4) | C18—Fe2—C21—C22 | 38.8 (3) |
C5—Fe1—C4—C3 | −120.4 (5) | C19iii—Fe2—C21—C22 | −96.6 (4) |
C5ii—Fe1—C4—C3 | 59.6 (5) | C19—Fe2—C21—C22 | 83.4 (4) |
C2—Fe1—C4—C3 | −37.5 (3) | C22iii—Fe2—C21—C22 | 180.0 |
C2ii—Fe1—C4—C3 | 142.5 (3) | C20iii—Fe2—C21—C22 | −60.2 (5) |
C3ii—Fe1—C4—C3 | 180.000 (1) | C20—Fe2—C21—C22 | 119.8 (5) |
C3—C4—C5—C1 | 0.1 (6) | C20—C21—C22—C18 | 0.3 (7) |
Fe1—C4—C5—C1 | −58.6 (4) | Fe2—C21—C22—C18 | −59.2 (4) |
C3—C4—C5—Fe1 | 58.7 (4) | C20—C21—C22—Fe2 | 59.5 (4) |
C2—C1—C5—C4 | −0.9 (6) | C19—C18—C22—C21 | 0.4 (7) |
P1—C1—C5—C4 | −175.6 (4) | P2—C18—C22—C21 | −175.9 (5) |
Fe1—C1—C5—C4 | 60.2 (4) | Fe2—C18—C22—C21 | 60.2 (4) |
C2—C1—C5—Fe1 | −61.1 (4) | C19—C18—C22—Fe2 | −59.9 (4) |
P1—C1—C5—Fe1 | 124.2 (4) | P2—C18—C22—Fe2 | 123.9 (5) |
C1ii—Fe1—C5—C4 | 61.1 (5) | C18iii—Fe2—C22—C21 | 62.3 (5) |
C1—Fe1—C5—C4 | −118.9 (5) | C18—Fe2—C22—C21 | −117.7 (5) |
C2—Fe1—C5—C4 | −80.5 (4) | C19iii—Fe2—C22—C21 | 100.1 (4) |
C2ii—Fe1—C5—C4 | 99.5 (4) | C19—Fe2—C22—C21 | −79.9 (4) |
C3—Fe1—C5—C4 | −36.7 (4) | C21iii—Fe2—C22—C21 | 180.0 |
C3ii—Fe1—C5—C4 | 143.3 (4) | C20iii—Fe2—C22—C21 | 142.9 (3) |
C4ii—Fe1—C5—C4 | 180.0 | C20—Fe2—C22—C21 | −37.1 (3) |
C1ii—Fe1—C5—C1 | 180.0 | C18iii—Fe2—C22—C18 | 180.0 |
C2—Fe1—C5—C1 | 38.4 (3) | C19iii—Fe2—C22—C18 | −142.1 (3) |
C2ii—Fe1—C5—C1 | −141.6 (3) | C19—Fe2—C22—C18 | 37.9 (3) |
C3—Fe1—C5—C1 | 82.2 (4) | C21iii—Fe2—C22—C18 | −62.3 (5) |
C3ii—Fe1—C5—C1 | −97.8 (4) | C21—Fe2—C22—C18 | 117.7 (5) |
C4—Fe1—C5—C1 | 118.9 (5) | C20iii—Fe2—C22—C18 | −99.3 (4) |
C4ii—Fe1—C5—C1 | −61.1 (5) | C20—Fe2—C22—C18 | 80.7 (4) |
C1—P1—C6—C7 | 169.3 (7) | C18—P2—C23—C28 | 156.4 (5) |
C12—P1—C6—C7 | 43.7 (7) | C29—P2—C23—C28 | −75.4 (6) |
C1—P1—C6—C11 | −16.2 (7) | C18—P2—C23—C24 | −22.8 (7) |
C12—P1—C6—C11 | −141.8 (6) | C29—P2—C23—C24 | 105.4 (6) |
C11—C6—C7—C8 | 5.6 (14) | C28—C23—C24—C25 | −1.2 (11) |
P1—C6—C7—C8 | −179.9 (8) | P2—C23—C24—C25 | 178.0 (7) |
C6—C7—C8—C9 | −2.0 (17) | C23—C24—C25—C26 | 0.3 (14) |
C7—C8—C9—C10 | −1.7 (17) | C24—C25—C26—C27 | 1.3 (15) |
C8—C9—C10—C11 | 1.8 (17) | C25—C26—C27—C28 | −1.8 (14) |
C7—C6—C11—C10 | −5.4 (13) | C26—C27—C28—C23 | 0.9 (12) |
P1—C6—C11—C10 | 179.9 (7) | C24—C23—C28—C27 | 0.6 (11) |
C9—C10—C11—C6 | 1.9 (16) | P2—C23—C28—C27 | −178.6 (6) |
C1—P1—C12—C13 | −70.6 (6) | C18—P2—C29—C34 | 70.2 (6) |
C6—P1—C12—C13 | 50.8 (6) | C23—P2—C29—C34 | −55.8 (6) |
C1—P1—C12—C17 | 107.1 (5) | C18—P2—C29—C30 | −108.1 (5) |
C6—P1—C12—C17 | −131.5 (5) | C23—P2—C29—C30 | 125.9 (5) |
C17—C12—C13—C14 | −0.5 (10) | C34—C29—C30—C31 | 0.7 (10) |
P1—C12—C13—C14 | 177.2 (6) | P2—C29—C30—C31 | 179.1 (5) |
C12—C13—C14—C15 | 1.6 (12) | C29—C30—C31—C32 | −1.1 (12) |
C13—C14—C15—C16 | −2.1 (14) | C30—C31—C32—C33 | −1.0 (14) |
C14—C15—C16—C17 | 1.5 (14) | C31—C32—C33—C34 | 3.4 (14) |
C15—C16—C17—C12 | −0.3 (12) | C30—C29—C34—C33 | 1.7 (11) |
C13—C12—C17—C16 | −0.1 (10) | P2—C29—C34—C33 | −176.6 (6) |
P1—C12—C17—C16 | −177.9 (6) | C32—C33—C34—C29 | −3.7 (13) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x, −y, −z+1; (iii) −x, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2A···Cl6ii | 0.98 | 2.85 | 3.829 (6) | 173 |
C13—H13A···Cl6ii | 0.93 | 2.87 | 3.671 (7) | 145 |
C27—H27A···Cl3 | 0.93 | 2.84 | 3.508 (8) | 130 |
C3—H3A···Cl1ii | 0.98 | 2.83 | 3.582 (7) | 134 |
C9—H9A···Cl5iv | 0.93 | 2.83 | 3.744 (9) | 168 |
C19—H19A···Cl2v | 0.98 | 2.87 | 3.564 (6) | 128 |
C21—H21A···Cl8vi | 0.98 | 2.83 | 3.582 (6) | 134 |
C28—H28A···Cl5v | 0.93 | 2.81 | 3.679 (7) | 155 |
C22—H22A···Cl4vi | 0.98 | 2.66 | 3.636 (6) | 173 |
Symmetry codes: (ii) −x, −y, −z+1; (iv) x+1/2, −y+1/2, z−1/2; (v) x−1/2, −y+1/2, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | 2[Fe(C17H14P)2]·[Sb4Cl16]·C2H6O |
Mr | 2208.98 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 11.6280 (3), 15.0898 (3), 25.6100 (6) |
β (°) | 90.342 (1) |
V (Å3) | 4493.56 (18) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.08 |
Crystal size (mm) | 0.34 × 0.22 × 0.20 |
Data collection | |
Diffractometer | Siemens SMART CCD area-detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.538, 0.681 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 25353, 7901, 5408 |
Rint | 0.084 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.042, 0.108, 0.96 |
No. of reflections | 7901 |
No. of parameters | 454 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.70, −1.01 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXTL (Sheldrick, 1997), SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990).
P1—C1 | 1.764 (6) | Sb1—Cl4 | 2.743 (2) |
P1—C6 | 1.792 (6) | Sb1—Cl8i | 3.012 (2) |
P1—C12 | 1.793 (6) | Sb1—Cl8 | 3.227 (2) |
P2—C18 | 1.776 (6) | Sb2—Cl5 | 2.397 (2) |
P2—C29 | 1.782 (6) | Sb2—Cl7 | 2.442 (2) |
P2—C23 | 1.800 (6) | Sb2—Cl6 | 2.462 (2) |
Sb1—Cl3 | 2.402 (2) | Sb2—Cl8 | 2.869 (2) |
Sb1—Cl2 | 2.431 (2) | Sb2—Cl4i | 2.949 (2) |
Sb1—Cl1 | 2.547 (2) | Sb2—Cl1 | 3.329 (2) |
Cl1—Sb1—Cl4 | 174.18 (5) | Cl6—Sb2—Cl8 | 177.21 (5) |
Cl2—Sb1—Cl8i | 177.24 (6) | Cl7—Sb2—Cl4i | 173.11 (6) |
Cl3—Sb1—Cl8 | 170.37 (5) | Cl5—Sb2—Cl1 | 164.68 (5) |
Symmetry code: (i) −x, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C2—H2A···Cl6ii | 0.98 | 2.85 | 3.829 (6) | 173 |
C13—H13A···Cl6ii | 0.93 | 2.87 | 3.671 (7) | 145 |
C27—H27A···Cl3 | 0.93 | 2.84 | 3.508 (8) | 130 |
C3—H3A···Cl1ii | 0.98 | 2.83 | 3.582 (7) | 134 |
C9—H9A···Cl5iii | 0.93 | 2.83 | 3.744 (9) | 168 |
C19—H19A···Cl2iv | 0.98 | 2.87 | 3.564 (6) | 128 |
C21—H21A···Cl8v | 0.98 | 2.83 | 3.582 (6) | 134 |
C28—H28A···Cl5iv | 0.93 | 2.81 | 3.679 (7) | 155 |
C22—H22A···Cl4v | 0.98 | 2.66 | 3.636 (6) | 173 |
Symmetry codes: (ii) −x, −y, −z+1; (iii) x+1/2, −y+1/2, z−1/2; (iv) x−1/2, −y+1/2, z−1/2; (v) −x+1/2, y−1/2, −z+1/2. |
Antimony trichloride is known to form adducts with phosphorus oxide derivatives such as triphenylphosphine oxide (Golic & Milicev, 1978). It also interacts with and oxidizes ferrocene in chloroform or acetonitrile to give ferrocenium tetrachloroantimonate (Yamin et al., 1996) and bis(ferrocenium) bis[tetrachloroantimonate(III)] trichloroantimony(III) (Razak et al., 2000), respectively. The presence of the P atom in diphenylphosphinoferrocene (dppf) was thought to give a P—Sb or Sb—O—P bond formation, as in case of dppf with SbCl4 or SbBr4 (Yamin et al., 1996). A good quality crystal of the title compound, (I), obtained from a mixture of dppf and SbCl3 in chloroform solution, was subjected to X-ray crystallographic investigation and the results are presented here. \sch
The asymmetric unit of (I) contains two [Fe{C5H4P(C6H5)2}2]2+ cations with the Fe atoms lying on inversion centres, an anionic [Sb4Cl16]4- cluster and one ethanol molecule (Fig. 1).
The C—C, Fe—C and Fe-centroid distances in the ferrocenium moieties are comparable with the values reported by Orpen et al. (1989) and Razak et al. (1998). The Sb—Cl bond lengths range from 2.397 (2) to 2.743 (2) Å. A very similar Sb—Cl range was also observed in a related structure (Razak et al., 2000). The longer bond lengths involving Cl1 and Cl4 are bridging, while the remaining Cl atoms are non-bridging (Porter & Jacobson, 1970; Yamin et al., 1996; Razak et al., 2000). The P—C bond lengths are comparable with the corresponding values in the structure reported by Carmalt et al. (1996), but the CPh—P—CPh bond angles in (I) are larger.
The cyclopentadienyl (Cp) rings are in a staggered conformation. The torsion angle between a ring C atom, the two ring centres and the corresponding C atom on the opposite ring defines the angle of twist for the Cp rings (Palenik, 1970). The average Cn—Cg···Cg'-Cn' (Cg is the ring centroid) torsion angle is 36° for both cations. Examples of the staggered and eclipsed conformations of Cp rings are given by Osborne et al. (1996).
Coordination around Sb1 is provided by atoms Cl1, Cl3, Cl4 and Cl8 at the equatorial positions, while the apices are occupied by Cl2 and Cl8i [symmetry code: (i) 1 - x, -y, -z Is this the correct symmetry code?]. The basal plane around Sb2 is formed by atoms Cl1, Cl5, Cl6 and Cl8, while the axial positions are occupied by Cl7 and Cl4i. The bond lengths and angles around the Sb atoms are in the ranges 2.397 (2)–3.329 (2) Å and 77.22 (4)–177.24 (6)°, respectively.
In the structure of (I), four SbCl4- form a Cl1—Cl8 edge-shared octahedron, to form an anionic centrosymmetric [Sb4Cl16]-4 cluster. Each cluster is surrounded by [Fe{C5H4P(C6H5)2}2]2+ cations. These formations are held together by weak C—H···Cl interactions and are joined continously along the a axis to form columns. These columns are then interconnected along the b axis by other C—H···Cl interactions (Table 2).