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In the title compound, [Fe(C
34H
29O
2P
2)]
2[Sb
2Cl
8], the discrete centrosymmetric [Sb
2Cl
8]
2− anions are formed from two edge-shared square pyramids of Cl atoms about each Sb atom. Within the cation, the two diphenylphosphinate groups share one H atom and the ferrocene cyclopentadienyl rings are in a staggered conformation, with the average value of the twist angle being 46°. In the crystal, each [Sb
2Cl
8]
2− anion is involved in eight C—H
Cl interactions with four surrounding cations and these interactions interconnect the ions to form molecular columns along the
a direction.
Supporting information
CCDC reference: 184464
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: XSCANS; 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).
Bis-[hydrogen-1,1'-bis(diphenylphosphinato)ferrocenium octachlorodiantimony(III)
top
Crystal data top
[Fe(C17H14OP)(C17H15OP)]2[Sb2Cl8] | Z = 1 |
Mr = 1701.82 | F(000) = 848 |
Triclinic, P1 | Dx = 1.634 Mg m−3 |
a = 11.036 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.348 (1) Å | Cell parameters from 38 reflections |
c = 14.002 (1) Å | θ = 5.3–12.5° |
α = 76.35 (1)° | µ = 1.63 mm−1 |
β = 77.19 (1)° | T = 293 K |
γ = 70.82 (1)° | Block, orange |
V = 1729.5 (2) Å3 | 0.38 × 0.36 × 0.32 mm |
Data collection top
Siemens P4 diffractometer | Rint = 0.015 |
Radiation source: fine-focus sealed tube | θmax = 25.0°, θmin = 1.5° |
Graphite monochromator | h = −1→13 |
θ/2θ scans | k = −13→14 |
7093 measured reflections | l = −16→16 |
6061 independent reflections | 3 standard reflections every 97 reflections |
5393 reflections with I > 2σ(I) | intensity decay: <3% |
Refinement top
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.076 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0408P)2 + 0.4246P] where P = (Fo2 + 2Fc2)/3 |
6061 reflections | (Δ/σ)max = 0.001 |
397 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.57 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sb1 | 0.346367 (17) | 0.494629 (16) | 0.431497 (12) | 0.04230 (7) | |
Fe1 | 0.44597 (3) | 0.04786 (3) | 0.74535 (2) | 0.03479 (9) | |
Cl1 | 0.47974 (9) | 0.46892 (10) | 0.27497 (6) | 0.0753 (3) | |
Cl2 | 0.55078 (9) | 0.33533 (7) | 0.52163 (7) | 0.0711 (2) | |
Cl3 | 0.19062 (9) | 0.66469 (8) | 0.34398 (7) | 0.0708 (2) | |
Cl4 | 0.24868 (8) | 0.34507 (7) | 0.42400 (6) | 0.05843 (19) | |
O1 | 0.12967 (19) | 0.16975 (16) | 0.92034 (14) | 0.0477 (4) | |
H1O | 0.1010 | 0.1225 | 0.8687 | 0.071* | |
O2 | 0.07619 (19) | 0.06682 (16) | 0.81671 (16) | 0.0516 (5) | |
P1 | 0.22681 (6) | 0.23927 (5) | 0.88716 (5) | 0.03564 (14) | |
P2 | 0.17185 (7) | −0.04337 (6) | 0.78236 (5) | 0.04031 (15) | |
C1 | 0.2340 (3) | 0.2969 (2) | 0.99160 (18) | 0.0421 (6) | |
C2 | 0.1186 (4) | 0.3394 (3) | 1.0520 (2) | 0.0693 (10) | |
H2A | 0.0403 | 0.3390 | 1.0378 | 0.083* | |
C3 | 0.1207 (5) | 0.3827 (4) | 1.1344 (3) | 0.0950 (14) | |
H3A | 0.0436 | 0.4108 | 1.1759 | 0.114* | |
C4 | 0.2357 (5) | 0.3843 (3) | 1.1549 (2) | 0.0780 (11) | |
H4A | 0.2364 | 0.4135 | 1.2101 | 0.094* | |
C5 | 0.3482 (4) | 0.3436 (3) | 1.0949 (2) | 0.0667 (9) | |
H5A | 0.4260 | 0.3450 | 1.1093 | 0.080* | |
C6 | 0.3489 (3) | 0.2995 (2) | 1.0123 (2) | 0.0518 (7) | |
H6A | 0.4267 | 0.2720 | 0.9712 | 0.062* | |
C7 | 0.1811 (2) | 0.3584 (2) | 0.78847 (18) | 0.0372 (5) | |
C8 | 0.2380 (3) | 0.4482 (2) | 0.7655 (2) | 0.0466 (6) | |
H8A | 0.2987 | 0.4474 | 0.8025 | 0.056* | |
C9 | 0.2042 (3) | 0.5389 (3) | 0.6876 (2) | 0.0526 (7) | |
H9A | 0.2435 | 0.5983 | 0.6714 | 0.063* | |
C10 | 0.1129 (3) | 0.5413 (2) | 0.6342 (2) | 0.0512 (7) | |
H10A | 0.0889 | 0.6034 | 0.5829 | 0.061* | |
C11 | 0.0568 (3) | 0.4523 (3) | 0.6561 (2) | 0.0524 (7) | |
H11A | −0.0034 | 0.4536 | 0.6184 | 0.063* | |
C12 | 0.0890 (3) | 0.3614 (2) | 0.7334 (2) | 0.0453 (6) | |
H12A | 0.0494 | 0.3022 | 0.7488 | 0.054* | |
C13 | 0.5716 (3) | −0.0013 (3) | 0.8463 (2) | 0.0497 (7) | |
H13A | 0.6332 | −0.0787 | 0.8608 | 0.060* | |
C14 | 0.4420 (3) | 0.0338 (2) | 0.89362 (18) | 0.0426 (6) | |
H14A | 0.3985 | −0.0137 | 0.9475 | 0.051* | |
C15 | 0.3854 (3) | 0.1530 (2) | 0.84899 (17) | 0.0373 (5) | |
C16 | 0.4835 (3) | 0.1875 (2) | 0.77422 (19) | 0.0427 (6) | |
H16A | 0.4735 | 0.2639 | 0.7309 | 0.051* | |
C17 | 0.5976 (3) | 0.0921 (3) | 0.7737 (2) | 0.0499 (7) | |
H17A | 0.6800 | 0.0905 | 0.7291 | 0.060* | |
C18 | 0.3213 (3) | 0.0899 (2) | 0.64475 (18) | 0.0431 (6) | |
H18A | 0.2483 | 0.1609 | 0.6362 | 0.052* | |
C19 | 0.4488 (3) | 0.0751 (3) | 0.59427 (19) | 0.0520 (7) | |
H19A | 0.4804 | 0.1346 | 0.5449 | 0.062* | |
C20 | 0.5247 (3) | −0.0393 (3) | 0.6277 (2) | 0.0521 (7) | |
H20A | 0.6176 | −0.0723 | 0.6052 | 0.063* | |
C21 | 0.4447 (3) | −0.0974 (2) | 0.6994 (2) | 0.0458 (6) | |
H21A | 0.4719 | −0.1778 | 0.7349 | 0.055* | |
C22 | 0.3162 (3) | −0.0174 (2) | 0.71166 (18) | 0.0389 (5) | |
C23 | 0.2097 (3) | −0.1571 (2) | 0.8866 (2) | 0.0440 (6) | |
C24 | 0.1907 (3) | −0.1302 (3) | 0.9800 (2) | 0.0581 (8) | |
H24A | 0.1559 | −0.0529 | 0.9886 | 0.070* | |
C25 | 0.2227 (4) | −0.2166 (3) | 1.0607 (2) | 0.0720 (10) | |
H25A | 0.2094 | −0.1980 | 1.1235 | 0.086* | |
C26 | 0.2745 (4) | −0.3307 (3) | 1.0475 (3) | 0.0775 (11) | |
H26A | 0.2980 | −0.3893 | 1.1014 | 0.093* | |
C27 | 0.2915 (5) | −0.3583 (3) | 0.9564 (3) | 0.0893 (14) | |
H27A | 0.3254 | −0.4359 | 0.9489 | 0.107* | |
C28 | 0.2596 (4) | −0.2736 (3) | 0.8748 (3) | 0.0686 (10) | |
H28A | 0.2711 | −0.2937 | 0.8127 | 0.082* | |
C29 | 0.0972 (3) | −0.0886 (2) | 0.7035 (2) | 0.0478 (6) | |
C30 | 0.1620 (4) | −0.1169 (3) | 0.6127 (2) | 0.0599 (8) | |
H30A | 0.2476 | −0.1154 | 0.5917 | 0.072* | |
C31 | 0.0984 (4) | −0.1480 (3) | 0.5521 (3) | 0.0730 (10) | |
H31A | 0.1412 | −0.1653 | 0.4900 | 0.088* | |
C32 | −0.0260 (4) | −0.1530 (3) | 0.5835 (3) | 0.0760 (11) | |
H32A | −0.0677 | −0.1740 | 0.5429 | 0.091* | |
C33 | −0.0891 (4) | −0.1274 (4) | 0.6742 (4) | 0.0918 (14) | |
H33A | −0.1735 | −0.1320 | 0.6956 | 0.110* | |
C34 | −0.0289 (4) | −0.0945 (4) | 0.7353 (3) | 0.0765 (11) | |
H34A | −0.0729 | −0.0765 | 0.7970 | 0.092* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sb1 | 0.04501 (11) | 0.05326 (12) | 0.03554 (11) | −0.02040 (8) | −0.01200 (8) | −0.00690 (8) |
Fe1 | 0.0443 (2) | 0.03503 (18) | 0.02582 (17) | −0.00871 (15) | −0.00742 (14) | −0.00914 (13) |
Cl1 | 0.0615 (5) | 0.1201 (8) | 0.0498 (4) | −0.0379 (5) | 0.0044 (4) | −0.0211 (5) |
Cl2 | 0.0706 (5) | 0.0593 (5) | 0.0828 (6) | −0.0259 (4) | −0.0226 (5) | 0.0082 (4) |
Cl3 | 0.0760 (6) | 0.0667 (5) | 0.0749 (6) | −0.0204 (4) | −0.0378 (5) | 0.0013 (4) |
Cl4 | 0.0627 (5) | 0.0584 (4) | 0.0642 (5) | −0.0263 (4) | −0.0201 (4) | −0.0081 (3) |
O1 | 0.0577 (12) | 0.0445 (10) | 0.0458 (10) | −0.0223 (9) | 0.0021 (9) | −0.0163 (8) |
O2 | 0.0523 (11) | 0.0430 (10) | 0.0633 (13) | −0.0101 (9) | −0.0117 (10) | −0.0198 (9) |
P1 | 0.0453 (4) | 0.0345 (3) | 0.0298 (3) | −0.0121 (3) | −0.0052 (3) | −0.0110 (2) |
P2 | 0.0490 (4) | 0.0340 (3) | 0.0419 (4) | −0.0120 (3) | −0.0117 (3) | −0.0101 (3) |
C1 | 0.0602 (17) | 0.0362 (13) | 0.0293 (12) | −0.0116 (12) | −0.0062 (11) | −0.0092 (10) |
C2 | 0.073 (2) | 0.090 (2) | 0.0542 (19) | −0.0270 (19) | 0.0068 (17) | −0.0402 (18) |
C3 | 0.118 (4) | 0.119 (4) | 0.057 (2) | −0.042 (3) | 0.020 (2) | −0.055 (2) |
C4 | 0.135 (4) | 0.077 (2) | 0.0360 (17) | −0.041 (2) | −0.017 (2) | −0.0200 (16) |
C5 | 0.101 (3) | 0.0555 (18) | 0.0565 (19) | −0.0235 (18) | −0.040 (2) | −0.0085 (15) |
C6 | 0.0659 (19) | 0.0449 (15) | 0.0493 (16) | −0.0118 (14) | −0.0187 (14) | −0.0142 (12) |
C7 | 0.0412 (13) | 0.0373 (12) | 0.0338 (12) | −0.0086 (11) | −0.0062 (10) | −0.0113 (10) |
C8 | 0.0526 (16) | 0.0476 (15) | 0.0464 (15) | −0.0205 (13) | −0.0152 (12) | −0.0057 (12) |
C9 | 0.0628 (18) | 0.0457 (15) | 0.0502 (17) | −0.0207 (14) | −0.0090 (14) | −0.0029 (12) |
C10 | 0.0583 (17) | 0.0446 (15) | 0.0415 (15) | −0.0034 (13) | −0.0095 (13) | −0.0049 (12) |
C11 | 0.0521 (16) | 0.0563 (17) | 0.0486 (16) | −0.0042 (14) | −0.0207 (13) | −0.0134 (13) |
C12 | 0.0483 (15) | 0.0454 (14) | 0.0478 (15) | −0.0137 (12) | −0.0130 (12) | −0.0137 (12) |
C13 | 0.0531 (16) | 0.0518 (16) | 0.0439 (15) | −0.0007 (13) | −0.0204 (13) | −0.0167 (12) |
C14 | 0.0600 (17) | 0.0424 (14) | 0.0271 (12) | −0.0106 (12) | −0.0143 (11) | −0.0084 (10) |
C15 | 0.0493 (14) | 0.0384 (13) | 0.0278 (11) | −0.0114 (11) | −0.0099 (10) | −0.0109 (10) |
C16 | 0.0528 (15) | 0.0427 (14) | 0.0383 (13) | −0.0175 (12) | −0.0076 (12) | −0.0125 (11) |
C17 | 0.0447 (15) | 0.0604 (17) | 0.0513 (16) | −0.0151 (13) | −0.0076 (12) | −0.0228 (13) |
C18 | 0.0635 (17) | 0.0397 (13) | 0.0314 (12) | −0.0156 (12) | −0.0162 (12) | −0.0068 (10) |
C19 | 0.079 (2) | 0.0595 (17) | 0.0259 (13) | −0.0287 (16) | −0.0092 (13) | −0.0108 (12) |
C20 | 0.0594 (18) | 0.0634 (18) | 0.0400 (14) | −0.0170 (15) | −0.0008 (13) | −0.0293 (13) |
C21 | 0.0587 (17) | 0.0384 (13) | 0.0436 (14) | −0.0082 (12) | −0.0142 (12) | −0.0162 (11) |
C22 | 0.0514 (15) | 0.0351 (12) | 0.0342 (13) | −0.0108 (11) | −0.0133 (11) | −0.0102 (10) |
C23 | 0.0541 (16) | 0.0389 (13) | 0.0422 (14) | −0.0185 (12) | −0.0078 (12) | −0.0059 (11) |
C24 | 0.082 (2) | 0.0494 (16) | 0.0441 (16) | −0.0236 (16) | −0.0036 (15) | −0.0109 (13) |
C25 | 0.104 (3) | 0.070 (2) | 0.0443 (18) | −0.034 (2) | −0.0106 (18) | −0.0033 (15) |
C26 | 0.111 (3) | 0.063 (2) | 0.056 (2) | −0.030 (2) | −0.024 (2) | 0.0118 (16) |
C27 | 0.145 (4) | 0.0410 (18) | 0.068 (2) | −0.010 (2) | −0.024 (3) | −0.0022 (16) |
C28 | 0.108 (3) | 0.0423 (16) | 0.0526 (18) | −0.0132 (17) | −0.0184 (18) | −0.0096 (13) |
C29 | 0.0580 (17) | 0.0355 (13) | 0.0559 (17) | −0.0117 (12) | −0.0218 (14) | −0.0103 (12) |
C30 | 0.075 (2) | 0.0605 (18) | 0.0568 (18) | −0.0267 (16) | −0.0187 (16) | −0.0171 (15) |
C31 | 0.110 (3) | 0.062 (2) | 0.063 (2) | −0.029 (2) | −0.034 (2) | −0.0173 (16) |
C32 | 0.091 (3) | 0.0496 (18) | 0.107 (3) | −0.0094 (18) | −0.062 (2) | −0.0226 (19) |
C33 | 0.064 (2) | 0.099 (3) | 0.134 (4) | −0.021 (2) | −0.035 (3) | −0.049 (3) |
C34 | 0.060 (2) | 0.093 (3) | 0.092 (3) | −0.0202 (19) | −0.0146 (19) | −0.047 (2) |
Geometric parameters (Å, º) top
Sb1—Cl1 | 2.379 (1) | C10—H10A | 0.9300 |
Sb1—Cl4 | 2.456 (1) | C11—C12 | 1.376 (4) |
Sb1—Cl3 | 2.493 (1) | C11—H11A | 0.9300 |
Sb1—Cl2 | 2.780 (1) | C12—H12A | 0.9300 |
Sb1—Cl2i | 2.945 (1) | C13—C14 | 1.406 (4) |
Fe1—C15 | 2.031 (2) | C13—C17 | 1.407 (4) |
Fe1—C14 | 2.034 (2) | C13—H13A | 0.9800 |
Fe1—C22 | 2.039 (3) | C14—C15 | 1.443 (4) |
Fe1—C16 | 2.044 (3) | C14—H14A | 0.9800 |
Fe1—C18 | 2.048 (3) | C15—C16 | 1.428 (4) |
Fe1—C21 | 2.048 (3) | C16—C17 | 1.414 (4) |
Fe1—C13 | 2.049 (3) | C16—H16A | 0.9800 |
Fe1—C20 | 2.053 (3) | C17—H17A | 0.9800 |
Fe1—C19 | 2.057 (3) | C18—C19 | 1.402 (4) |
Fe1—C17 | 2.062 (3) | C18—C22 | 1.441 (3) |
Cl2—Sb1i | 2.9452 (10) | C18—H18A | 0.9800 |
O1—P1 | 1.5158 (19) | C19—C20 | 1.414 (4) |
O1—H1O | 1.1771 (18) | C19—H19A | 0.9800 |
O2—P2 | 1.529 (2) | C20—C21 | 1.409 (4) |
O2—H1O | 1.2352 (19) | C20—H20A | 0.9800 |
P1—C15 | 1.764 (3) | C21—C22 | 1.438 (4) |
P1—C7 | 1.786 (3) | C21—H21A | 0.9800 |
P1—C1 | 1.797 (3) | C23—C24 | 1.379 (4) |
P2—C22 | 1.763 (3) | C23—C28 | 1.397 (4) |
P2—C23 | 1.787 (3) | C24—C25 | 1.379 (5) |
P2—C29 | 1.791 (3) | C24—H24A | 0.9300 |
C1—C6 | 1.374 (4) | C25—C26 | 1.376 (5) |
C1—C2 | 1.381 (4) | C25—H25A | 0.9300 |
C2—C3 | 1.389 (5) | C26—C27 | 1.354 (5) |
C2—H2A | 0.9300 | C26—H26A | 0.9300 |
C3—C4 | 1.368 (6) | C27—C28 | 1.377 (5) |
C3—H3A | 0.9300 | C27—H27A | 0.9300 |
C4—C5 | 1.351 (6) | C28—H28A | 0.9300 |
C4—H4A | 0.9300 | C29—C30 | 1.377 (4) |
C5—C6 | 1.387 (4) | C29—C34 | 1.383 (5) |
C5—H5A | 0.9300 | C30—C31 | 1.398 (4) |
C6—H6A | 0.9300 | C30—H30A | 0.9300 |
C7—C8 | 1.388 (4) | C31—C32 | 1.362 (6) |
C7—C12 | 1.393 (4) | C31—H31A | 0.9300 |
C8—C9 | 1.383 (4) | C32—C33 | 1.360 (6) |
C8—H8A | 0.9300 | C32—H32A | 0.9300 |
C9—C10 | 1.370 (4) | C33—C34 | 1.391 (5) |
C9—H9A | 0.9300 | C33—H33A | 0.9300 |
C10—C11 | 1.375 (4) | C34—H34A | 0.9300 |
| | | |
Cl1—Sb1—Cl4 | 90.96 (3) | C10—C11—H11A | 119.8 |
Cl1—Sb1—Cl3 | 88.79 (4) | C12—C11—H11A | 119.8 |
Cl4—Sb1—Cl3 | 97.34 (3) | C11—C12—C7 | 119.7 (3) |
Cl1—Sb1—Cl2 | 88.00 (3) | C11—C12—H12A | 120.1 |
Cl4—Sb1—Cl2 | 93.86 (3) | C7—C12—H12A | 120.1 |
Cl3—Sb1—Cl2 | 168.40 (3) | C14—C13—C17 | 109.0 (3) |
Cl1—Sb1—Cl2i | 98.29 (3) | C14—C13—Fe1 | 69.27 (15) |
Cl4—Sb1—Cl2i | 169.96 (3) | C17—C13—Fe1 | 70.49 (16) |
Cl3—Sb1—Cl2i | 86.79 (3) | C14—C13—H13A | 125.5 |
Cl2—Sb1—Cl2i | 82.64 (3) | C17—C13—H13A | 125.5 |
C15—Fe1—C14 | 41.57 (10) | Fe1—C13—H13A | 125.5 |
C15—Fe1—C22 | 119.16 (10) | C13—C14—C15 | 107.5 (2) |
C14—Fe1—C22 | 114.42 (11) | C13—C14—Fe1 | 70.43 (15) |
C15—Fe1—C16 | 41.02 (10) | C15—C14—Fe1 | 69.12 (13) |
C14—Fe1—C16 | 69.02 (11) | C13—C14—H14A | 126.2 |
C22—Fe1—C16 | 147.95 (11) | C15—C14—H14A | 126.2 |
C15—Fe1—C18 | 113.20 (11) | Fe1—C14—H14A | 126.2 |
C14—Fe1—C18 | 140.03 (11) | C16—C15—C14 | 107.2 (2) |
C22—Fe1—C18 | 41.29 (10) | C16—C15—P1 | 127.71 (19) |
C16—Fe1—C18 | 114.39 (11) | C14—C15—P1 | 125.0 (2) |
C15—Fe1—C21 | 149.49 (11) | C16—C15—Fe1 | 69.98 (14) |
C14—Fe1—C21 | 116.36 (11) | C14—C15—Fe1 | 69.31 (13) |
C22—Fe1—C21 | 41.19 (11) | P1—C15—Fe1 | 128.57 (14) |
C16—Fe1—C21 | 168.46 (12) | C17—C16—C15 | 107.9 (2) |
C18—Fe1—C21 | 68.76 (11) | C17—C16—Fe1 | 70.54 (16) |
C15—Fe1—C13 | 68.54 (11) | C15—C16—Fe1 | 69.00 (14) |
C14—Fe1—C13 | 40.29 (11) | C17—C16—H16A | 126.0 |
C22—Fe1—C13 | 136.65 (12) | C15—C16—H16A | 126.0 |
C16—Fe1—C13 | 67.96 (12) | Fe1—C16—H16A | 126.0 |
C18—Fe1—C13 | 177.65 (11) | C13—C17—C16 | 108.4 (3) |
C21—Fe1—C13 | 108.93 (11) | C13—C17—Fe1 | 69.48 (17) |
C15—Fe1—C20 | 170.31 (12) | C16—C17—Fe1 | 69.18 (16) |
C14—Fe1—C20 | 143.35 (12) | C13—C17—H17A | 125.8 |
C22—Fe1—C20 | 68.39 (11) | C16—C17—H17A | 125.8 |
C16—Fe1—C20 | 129.36 (12) | Fe1—C17—H17A | 125.8 |
C18—Fe1—C20 | 67.80 (12) | C19—C18—C22 | 108.1 (2) |
C21—Fe1—C20 | 40.20 (11) | C19—C18—Fe1 | 70.39 (16) |
C13—Fe1—C20 | 110.78 (12) | C22—C18—Fe1 | 69.05 (14) |
C15—Fe1—C19 | 134.40 (11) | C19—C18—H18A | 126.0 |
C14—Fe1—C19 | 175.68 (11) | C22—C18—H18A | 126.0 |
C22—Fe1—C19 | 68.33 (11) | Fe1—C18—H18A | 126.0 |
C16—Fe1—C19 | 106.84 (11) | C18—C19—C20 | 108.6 (3) |
C18—Fe1—C19 | 39.94 (12) | C18—C19—Fe1 | 69.68 (15) |
C21—Fe1—C19 | 67.94 (11) | C20—C19—Fe1 | 69.73 (15) |
C13—Fe1—C19 | 140.02 (13) | C18—C19—H19A | 125.7 |
C20—Fe1—C19 | 40.25 (12) | C20—C19—H19A | 125.7 |
C15—Fe1—C17 | 68.30 (11) | Fe1—C19—H19A | 125.7 |
C14—Fe1—C17 | 67.98 (12) | C21—C20—C19 | 108.7 (3) |
C22—Fe1—C17 | 171.57 (11) | C21—C20—Fe1 | 69.70 (15) |
C16—Fe1—C17 | 40.27 (11) | C19—C20—Fe1 | 70.02 (15) |
C18—Fe1—C17 | 141.77 (12) | C21—C20—H20A | 125.7 |
C21—Fe1—C17 | 130.39 (12) | C19—C20—H20A | 125.7 |
C13—Fe1—C17 | 40.02 (12) | Fe1—C20—H20A | 125.7 |
C20—Fe1—C17 | 104.67 (12) | C20—C21—C22 | 107.8 (2) |
C19—Fe1—C17 | 109.80 (12) | C20—C21—Fe1 | 70.10 (15) |
Sb1—Cl2—Sb1i | 97.36 (3) | C22—C21—Fe1 | 69.08 (14) |
P1—O1—H1O | 124.94 (14) | C20—C21—H21A | 126.1 |
P2—O2—H1O | 123.83 (15) | C22—C21—H21A | 126.1 |
O1—P1—C15 | 112.64 (11) | Fe1—C21—H21A | 126.1 |
O1—P1—C7 | 112.18 (12) | C21—C22—C18 | 106.9 (2) |
C15—P1—C7 | 108.56 (12) | C21—C22—P2 | 128.9 (2) |
O1—P1—C1 | 108.11 (12) | C18—C22—P2 | 123.9 (2) |
C15—P1—C1 | 106.84 (12) | C21—C22—Fe1 | 69.72 (15) |
C7—P1—C1 | 108.27 (11) | C18—C22—Fe1 | 69.67 (15) |
O2—P2—C22 | 111.80 (12) | P2—C22—Fe1 | 130.71 (13) |
O2—P2—C23 | 110.66 (13) | C24—C23—C28 | 119.2 (3) |
C22—P2—C23 | 109.62 (13) | C24—C23—P2 | 119.9 (2) |
O2—P2—C29 | 107.93 (12) | C28—C23—P2 | 120.8 (2) |
C22—P2—C29 | 107.35 (13) | C25—C24—C23 | 120.7 (3) |
C23—P2—C29 | 109.38 (13) | C25—C24—H24A | 119.7 |
C6—C1—C2 | 120.0 (3) | C23—C24—H24A | 119.7 |
C6—C1—P1 | 122.4 (2) | C26—C25—C24 | 119.5 (3) |
C2—C1—P1 | 117.6 (2) | C26—C25—H25A | 120.3 |
C1—C2—C3 | 119.2 (4) | C24—C25—H25A | 120.3 |
C1—C2—H2A | 120.4 | C27—C26—C25 | 120.3 (3) |
C3—C2—H2A | 120.4 | C27—C26—H26A | 119.8 |
C4—C3—C2 | 120.4 (4) | C25—C26—H26A | 119.8 |
C4—C3—H3A | 119.8 | C26—C27—C28 | 121.3 (3) |
C2—C3—H3A | 119.8 | C26—C27—H27A | 119.4 |
C5—C4—C3 | 120.1 (3) | C28—C27—H27A | 119.4 |
C5—C4—H4A | 119.9 | C27—C28—C23 | 119.0 (3) |
C3—C4—H4A | 119.9 | C27—C28—H28A | 120.5 |
C4—C5—C6 | 120.7 (4) | C23—C28—H28A | 120.5 |
C4—C5—H5A | 119.7 | C30—C29—C34 | 119.8 (3) |
C6—C5—H5A | 119.7 | C30—C29—P2 | 121.5 (2) |
C1—C6—C5 | 119.6 (3) | C34—C29—P2 | 118.7 (2) |
C1—C6—H6A | 120.2 | C29—C30—C31 | 119.6 (3) |
C5—C6—H6A | 120.2 | C29—C30—H30A | 120.2 |
C8—C7—C12 | 119.4 (2) | C31—C30—H30A | 120.2 |
C8—C7—P1 | 120.3 (2) | C32—C31—C30 | 120.4 (4) |
C12—C7—P1 | 120.3 (2) | C32—C31—H31A | 119.8 |
C9—C8—C7 | 120.0 (3) | C30—C31—H31A | 119.8 |
C9—C8—H8A | 120.0 | C33—C32—C31 | 120.0 (3) |
C7—C8—H8A | 120.0 | C33—C32—H32A | 120.0 |
C10—C9—C8 | 120.1 (3) | C31—C32—H32A | 120.0 |
C10—C9—H9A | 120.0 | C32—C33—C34 | 120.8 (4) |
C8—C9—H9A | 120.0 | C32—C33—H33A | 119.6 |
C9—C10—C11 | 120.3 (3) | C34—C33—H33A | 119.6 |
C9—C10—H10A | 119.9 | C29—C34—C33 | 119.4 (4) |
C11—C10—H10A | 119.9 | C29—C34—H34A | 120.3 |
C10—C11—C12 | 120.5 (3) | C33—C34—H34A | 120.3 |
| | | |
Cl1—Sb1—Cl2—Sb1i | 98.62 (3) | C19—Fe1—C17—C16 | 92.94 (18) |
Cl4—Sb1—Cl2—Sb1i | −170.55 (3) | C15—Fe1—C18—C19 | 132.37 (17) |
Cl3—Sb1—Cl2—Sb1i | 24.58 (17) | C14—Fe1—C18—C19 | 173.27 (17) |
O1—P1—C1—C6 | 139.4 (2) | C22—Fe1—C18—C19 | −119.3 (2) |
C15—P1—C1—C6 | 17.9 (3) | C16—Fe1—C18—C19 | 87.36 (18) |
C7—P1—C1—C6 | −98.9 (2) | C21—Fe1—C18—C19 | −80.60 (18) |
O1—P1—C1—C2 | −40.6 (3) | C20—Fe1—C18—C19 | −37.19 (17) |
C15—P1—C1—C2 | −162.1 (2) | C17—Fe1—C18—C19 | 48.4 (3) |
C7—P1—C1—C2 | 81.2 (3) | C15—Fe1—C18—C22 | −108.38 (16) |
C6—C1—C2—C3 | −1.1 (5) | C14—Fe1—C18—C22 | −67.5 (2) |
P1—C1—C2—C3 | 178.9 (3) | C16—Fe1—C18—C22 | −153.39 (15) |
C1—C2—C3—C4 | 0.6 (7) | C21—Fe1—C18—C22 | 38.66 (15) |
C2—C3—C4—C5 | 0.0 (7) | C20—Fe1—C18—C22 | 82.07 (17) |
C3—C4—C5—C6 | −0.1 (6) | C19—Fe1—C18—C22 | 119.3 (2) |
C2—C1—C6—C5 | 0.9 (4) | C17—Fe1—C18—C22 | 167.70 (17) |
P1—C1—C6—C5 | −179.0 (2) | C22—C18—C19—C20 | 0.1 (3) |
C4—C5—C6—C1 | −0.3 (5) | Fe1—C18—C19—C20 | 59.03 (19) |
O1—P1—C7—C8 | 163.5 (2) | C22—C18—C19—Fe1 | −58.98 (17) |
C15—P1—C7—C8 | −71.4 (2) | C15—Fe1—C19—C18 | −71.9 (2) |
C1—P1—C7—C8 | 44.3 (2) | C22—Fe1—C19—C18 | 38.27 (15) |
O1—P1—C7—C12 | −17.0 (2) | C16—Fe1—C19—C18 | −108.10 (17) |
C15—P1—C7—C12 | 108.1 (2) | C21—Fe1—C19—C18 | 82.82 (17) |
C1—P1—C7—C12 | −136.2 (2) | C13—Fe1—C19—C18 | 176.34 (17) |
C12—C7—C8—C9 | −0.9 (4) | C20—Fe1—C19—C18 | 120.0 (2) |
P1—C7—C8—C9 | 178.6 (2) | C17—Fe1—C19—C18 | −150.51 (16) |
C7—C8—C9—C10 | 1.2 (4) | C15—Fe1—C19—C20 | 168.12 (18) |
C8—C9—C10—C11 | −1.6 (4) | C22—Fe1—C19—C20 | −81.72 (19) |
C9—C10—C11—C12 | 1.7 (4) | C16—Fe1—C19—C20 | 131.91 (18) |
C10—C11—C12—C7 | −1.3 (4) | C18—Fe1—C19—C20 | −120.0 (2) |
C8—C7—C12—C11 | 0.9 (4) | C21—Fe1—C19—C20 | −37.17 (18) |
P1—C7—C12—C11 | −178.5 (2) | C13—Fe1—C19—C20 | 56.4 (3) |
C15—Fe1—C13—C14 | 38.80 (16) | C17—Fe1—C19—C20 | 89.50 (19) |
C22—Fe1—C13—C14 | −71.5 (2) | C18—C19—C20—C21 | 0.2 (3) |
C16—Fe1—C13—C14 | 83.12 (17) | Fe1—C19—C20—C21 | 59.18 (19) |
C21—Fe1—C13—C14 | −108.75 (17) | C18—C19—C20—Fe1 | −58.99 (18) |
C20—Fe1—C13—C14 | −151.56 (16) | C14—Fe1—C20—C21 | 64.0 (3) |
C19—Fe1—C13—C14 | 173.32 (17) | C22—Fe1—C20—C21 | −38.26 (16) |
C17—Fe1—C13—C14 | 120.2 (2) | C16—Fe1—C20—C21 | 173.07 (16) |
C15—Fe1—C13—C17 | −81.40 (17) | C18—Fe1—C20—C21 | −82.92 (18) |
C14—Fe1—C13—C17 | −120.2 (2) | C13—Fe1—C20—C21 | 95.07 (19) |
C22—Fe1—C13—C17 | 168.34 (16) | C19—Fe1—C20—C21 | −119.8 (3) |
C16—Fe1—C13—C17 | −37.08 (16) | C17—Fe1—C20—C21 | 136.71 (18) |
C21—Fe1—C13—C17 | 131.05 (17) | C14—Fe1—C20—C19 | −176.2 (2) |
C20—Fe1—C13—C17 | 88.24 (18) | C22—Fe1—C20—C19 | 81.57 (19) |
C19—Fe1—C13—C17 | 53.1 (2) | C16—Fe1—C20—C19 | −67.1 (2) |
C17—C13—C14—C15 | 0.1 (3) | C18—Fe1—C20—C19 | 36.91 (18) |
Fe1—C13—C14—C15 | −59.42 (17) | C21—Fe1—C20—C19 | 119.8 (3) |
C17—C13—C14—Fe1 | 59.49 (19) | C13—Fe1—C20—C19 | −145.10 (18) |
C15—Fe1—C14—C13 | −118.5 (2) | C17—Fe1—C20—C19 | −103.46 (19) |
C22—Fe1—C14—C13 | 134.37 (17) | C19—C20—C21—C22 | −0.4 (3) |
C16—Fe1—C14—C13 | −80.26 (18) | Fe1—C20—C21—C22 | 59.02 (17) |
C18—Fe1—C14—C13 | 176.39 (17) | C19—C20—C21—Fe1 | −59.38 (19) |
C21—Fe1—C14—C13 | 88.59 (19) | C15—Fe1—C21—C20 | −179.7 (2) |
C20—Fe1—C14—C13 | 48.2 (3) | C14—Fe1—C21—C20 | −143.21 (18) |
C17—Fe1—C14—C13 | −36.84 (17) | C22—Fe1—C21—C20 | 119.1 (2) |
C22—Fe1—C14—C15 | −107.13 (16) | C16—Fe1—C21—C20 | −27.8 (6) |
C16—Fe1—C14—C15 | 38.24 (16) | C18—Fe1—C21—C20 | 80.32 (18) |
C18—Fe1—C14—C15 | −65.1 (2) | C13—Fe1—C21—C20 | −100.10 (19) |
C21—Fe1—C14—C15 | −152.91 (16) | C19—Fe1—C21—C20 | 37.22 (18) |
C13—Fe1—C14—C15 | 118.5 (2) | C17—Fe1—C21—C20 | −60.6 (2) |
C20—Fe1—C14—C15 | 166.73 (19) | C15—Fe1—C21—C22 | 61.2 (3) |
C17—Fe1—C14—C15 | 81.66 (17) | C14—Fe1—C21—C22 | 97.72 (17) |
C13—C14—C15—C16 | 0.3 (3) | C16—Fe1—C21—C22 | −146.8 (5) |
Fe1—C14—C15—C16 | −60.01 (17) | C18—Fe1—C21—C22 | −38.74 (15) |
C13—C14—C15—P1 | −176.43 (19) | C13—Fe1—C21—C22 | 140.84 (16) |
Fe1—C14—C15—P1 | 123.31 (19) | C20—Fe1—C21—C22 | −119.1 (2) |
C13—C14—C15—Fe1 | 60.26 (18) | C19—Fe1—C21—C22 | −81.85 (17) |
O1—P1—C15—C16 | 147.9 (2) | C17—Fe1—C21—C22 | −179.62 (15) |
C7—P1—C15—C16 | 23.1 (3) | C20—C21—C22—C18 | 0.4 (3) |
C1—P1—C15—C16 | −93.5 (2) | Fe1—C21—C22—C18 | 60.04 (17) |
O1—P1—C15—C14 | −36.1 (2) | C20—C21—C22—P2 | 173.8 (2) |
C7—P1—C15—C14 | −161.0 (2) | Fe1—C21—C22—P2 | −126.5 (2) |
C1—P1—C15—C14 | 82.5 (2) | C20—C21—C22—Fe1 | −59.66 (18) |
O1—P1—C15—Fe1 | 54.30 (19) | C19—C18—C22—C21 | −0.3 (3) |
C7—P1—C15—Fe1 | −70.57 (19) | Fe1—C18—C22—C21 | −60.08 (17) |
C1—P1—C15—Fe1 | 172.87 (15) | C19—C18—C22—P2 | −174.10 (18) |
C14—Fe1—C15—C16 | 118.3 (2) | Fe1—C18—C22—P2 | 126.09 (19) |
C22—Fe1—C15—C16 | −146.87 (16) | C19—C18—C22—Fe1 | 59.81 (18) |
C18—Fe1—C15—C16 | −101.06 (17) | O2—P2—C22—C21 | 152.6 (2) |
C21—Fe1—C15—C16 | 171.8 (2) | C23—P2—C22—C21 | 29.5 (3) |
C13—Fe1—C15—C16 | 80.65 (17) | C29—P2—C22—C21 | −89.3 (2) |
C19—Fe1—C15—C16 | −59.5 (2) | O2—P2—C22—C18 | −35.0 (2) |
C17—Fe1—C15—C16 | 37.46 (17) | C23—P2—C22—C18 | −158.1 (2) |
C22—Fe1—C15—C14 | 94.84 (17) | C29—P2—C22—C18 | 83.2 (2) |
C16—Fe1—C15—C14 | −118.3 (2) | O2—P2—C22—Fe1 | 56.4 (2) |
C18—Fe1—C15—C14 | 140.65 (16) | C23—P2—C22—Fe1 | −66.6 (2) |
C21—Fe1—C15—C14 | 53.5 (3) | C29—P2—C22—Fe1 | 174.64 (16) |
C13—Fe1—C15—C14 | −37.64 (17) | C15—Fe1—C22—C21 | −149.37 (15) |
C19—Fe1—C15—C14 | −177.75 (18) | C14—Fe1—C22—C21 | −102.81 (17) |
C17—Fe1—C15—C14 | −80.82 (18) | C16—Fe1—C22—C21 | 168.10 (19) |
C14—Fe1—C15—P1 | −118.9 (2) | C18—Fe1—C22—C21 | 117.9 (2) |
C22—Fe1—C15—P1 | −24.0 (2) | C13—Fe1—C22—C21 | −60.5 (2) |
C16—Fe1—C15—P1 | 122.8 (2) | C20—Fe1—C22—C21 | 37.36 (16) |
C18—Fe1—C15—P1 | 21.8 (2) | C19—Fe1—C22—C21 | 80.81 (17) |
C21—Fe1—C15—P1 | −65.4 (3) | C15—Fe1—C22—C18 | 92.77 (17) |
C13—Fe1—C15—P1 | −156.5 (2) | C14—Fe1—C22—C18 | 139.33 (15) |
C19—Fe1—C15—P1 | 63.4 (2) | C16—Fe1—C22—C18 | 50.2 (3) |
C17—Fe1—C15—P1 | 160.3 (2) | C21—Fe1—C22—C18 | −117.9 (2) |
C14—C15—C16—C17 | −0.5 (3) | C13—Fe1—C22—C18 | −178.34 (16) |
P1—C15—C16—C17 | 176.10 (19) | C20—Fe1—C22—C18 | −80.51 (17) |
Fe1—C15—C16—C17 | −60.05 (18) | C19—Fe1—C22—C18 | −37.06 (16) |
C14—C15—C16—Fe1 | 59.58 (16) | C15—Fe1—C22—P2 | −25.0 (2) |
P1—C15—C16—Fe1 | −123.9 (2) | C14—Fe1—C22—P2 | 21.6 (2) |
C15—Fe1—C16—C17 | 119.0 (2) | C16—Fe1—C22—P2 | −67.5 (3) |
C14—Fe1—C16—C17 | 80.30 (18) | C18—Fe1—C22—P2 | −117.7 (2) |
C22—Fe1—C16—C17 | −176.88 (19) | C21—Fe1—C22—P2 | 124.4 (3) |
C18—Fe1—C16—C17 | −143.04 (18) | C13—Fe1—C22—P2 | 63.9 (2) |
C21—Fe1—C16—C17 | −39.6 (6) | C20—Fe1—C22—P2 | 161.7 (2) |
C13—Fe1—C16—C17 | 36.86 (17) | C19—Fe1—C22—P2 | −154.8 (2) |
C20—Fe1—C16—C17 | −62.5 (2) | O2—P2—C23—C24 | −21.1 (3) |
C19—Fe1—C16—C17 | −100.97 (19) | C22—P2—C23—C24 | 102.6 (3) |
C14—Fe1—C16—C15 | −38.74 (15) | C29—P2—C23—C24 | −139.9 (3) |
C22—Fe1—C16—C15 | 64.1 (2) | O2—P2—C23—C28 | 159.4 (3) |
C18—Fe1—C16—C15 | 97.92 (16) | C22—P2—C23—C28 | −76.8 (3) |
C21—Fe1—C16—C15 | −158.7 (5) | C29—P2—C23—C28 | 40.6 (3) |
C13—Fe1—C16—C15 | −82.18 (17) | C28—C23—C24—C25 | 1.3 (5) |
C20—Fe1—C16—C15 | 178.44 (16) | P2—C23—C24—C25 | −178.2 (3) |
C19—Fe1—C16—C15 | 139.98 (16) | C23—C24—C25—C26 | 0.2 (6) |
C17—Fe1—C16—C15 | −119.0 (2) | C24—C25—C26—C27 | −1.3 (7) |
C14—C13—C17—C16 | −0.4 (3) | C25—C26—C27—C28 | 1.0 (8) |
Fe1—C13—C17—C16 | 58.38 (19) | C26—C27—C28—C23 | 0.5 (7) |
C14—C13—C17—Fe1 | −58.74 (19) | C24—C23—C28—C27 | −1.6 (6) |
C15—C16—C17—C13 | 0.5 (3) | P2—C23—C28—C27 | 177.9 (3) |
Fe1—C16—C17—C13 | −58.57 (19) | O2—P2—C29—C30 | 131.8 (2) |
C15—C16—C17—Fe1 | 59.08 (17) | C22—P2—C29—C30 | 11.1 (3) |
C15—Fe1—C17—C13 | 82.03 (17) | C23—P2—C29—C30 | −107.8 (3) |
C14—Fe1—C17—C13 | 37.08 (16) | O2—P2—C29—C34 | −47.9 (3) |
C16—Fe1—C17—C13 | 120.2 (2) | C22—P2—C29—C34 | −168.6 (3) |
C18—Fe1—C17—C13 | −177.59 (17) | C23—P2—C29—C34 | 72.5 (3) |
C21—Fe1—C17—C13 | −69.5 (2) | C34—C29—C30—C31 | 1.9 (5) |
C20—Fe1—C17—C13 | −104.99 (18) | P2—C29—C30—C31 | −177.8 (2) |
C19—Fe1—C17—C13 | −146.89 (17) | C29—C30—C31—C32 | −1.5 (5) |
C15—Fe1—C17—C16 | −38.14 (16) | C30—C31—C32—C33 | 0.2 (6) |
C14—Fe1—C17—C16 | −83.09 (17) | C31—C32—C33—C34 | 0.9 (7) |
C18—Fe1—C17—C16 | 62.2 (2) | C30—C29—C34—C33 | −0.9 (6) |
C21—Fe1—C17—C16 | 170.36 (16) | P2—C29—C34—C33 | 178.8 (3) |
C13—Fe1—C17—C16 | −120.2 (2) | C32—C33—C34—C29 | −0.5 (7) |
C20—Fe1—C17—C16 | 134.84 (17) | | |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1O···O2 | 1.1771 (18) | 1.2352 (19) | 2.411 (3) | 176.19 (13) |
C19—H19A···Cl2 | 0.98 | 2.76 | 3.599 (4) | 144 |
C16—H16A···Cl2 | 0.98 | 2.87 | 3.615 (3) | 133 |
C8—H8A···Cl1i | 0.93 | 2.86 | 3.481 (4) | 125 |
C11—H11A···Cl3ii | 0.93 | 2.80 | 3.484 (4) | 132 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1. |
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