Two new structures from a very small group to date of six-coordinate monocationic iron(III) complexes containing two bidentate phosphane and two halido ligands are presented as dichloromethane solvates. The Fe—P and Fe—Cl bond lengths are longer and shorter, respectively, than those previously reported for cations in this group.
Keywords: iron, bidentate phosphane, inversion twin, crystal structure, iron-catalysed cross-coupling
Abstract
Structural characterization of the ionic complexes [FeCl2(C26H22P2)2][FeCl4]·0.59CH2Cl2 or [(dppen)2FeCl2][FeCl4]·0.59CH2Cl2 (dppen = cis-1,2-bis(diphenylphosphane)ethylene, P2C26H22) and [FeCl2(C30H24P2)2][FeCl4]·CH2Cl2 or [(dpbz)2FeCl2][FeCl4]·CH2Cl2 (dpbz = 1,2-bis(diphenylphosphane)benzene, P2C30H24) demonstrates trans coordination of two bidentate phosphane ligands (bisphosphanes) to a single iron(III) center, resulting in six-coordinate cationic complexes that are balanced in charge by tetrachloridoferrate(III) monoanions. The trans bisphosphane coordination is consistent will all previously reported molecular structures of six coordinate iron(III) complex cations with a (PP)2 X 2 (X = halido) donor set. The complex with dppen crystallizes in the centrosymmetric space group C2/c as a partial-occupancy [0.592 (4)] dichloromethane solvate, while the dpbz-ligated complex crystallizes in the triclinic space group P1 as a full dichloromethane monosolvate. Furthermore, the crystal studied of [(dpbz)2FeCl2][FeCl4]·CH2Cl2 was an inversion twin, whose component mass ratio refined to 0.76 (3):0.24 (3). Beyond a few very weak C—H⋯Cl and C—H⋯π interactions, there are no significant supramolecular features in either structure.
Chemical context
Bidentate phosphanes (bisphosphanes) are versatile supporting ligands in coordination chemistry because of the accessibility of various electronic and steric properties through manipulation of their backbone structures and phosphorus substituents. While these ligands are commonly used to stabilize low-valent metal complexes due to their function as both σ-donor and π-acceptor ligands, bisphosphane ligands have also been observed to support metal centers in higher oxidation states. For example, there exist a few structurally characterized examples of iron(III) complexes in which two bisphosphane ligands are coordinated to a single metal center, resulting in axial coordination of halido (X) ligands. These complex cations have been shown to be accessible through a variety of synthetic routes (Higgins et al., 1985 ▸; Higgins & Levason, 1985 ▸; Field et al., 1990 ▸, 2000 ▸; Evans et al., 1992 ▸; Miller et al., 2002 ▸; Hoffert et al., 2011 ▸). A review of the literature finds that investigations into these complexes date back almost sixty years to the work of Chatt and Hayter, in which three distinct iron(III) bisphosphane complexes, formulated as complex salts with the molecular structures [(PP)2FeCl2][FeCl4] [PP = 1,2-bis(diethylphosphano)benzene (debz), 1,2-bis(diethylphosphano)ethane (depe), and 1,2-bis(dimethylphosphano)ethane (dmpe)], were prepared through the reaction of iron(III) chloride with one shoichiometric equivalent of bisphosphane (Chatt & Hayter, 1961 ▸; for later reports of various preparative methods of similar compounds, see: Levason et al., 1975 ▸; Gargano et al., 1975 ▸; Warren et al., 1976 ▸; Higgins & Levason, 1985 ▸). Structural confirmation for this general molecular formula was achieved through the crystallographic characterization of [(dmpe)2FeCl2][FeCl4], although this synthesis employed photolytic oxidation of the iron(II) complex (dmpe)2FeCl2 and not direct reaction of an iron(III) precursor with bisphosphane (Field et al., 1990 ▸). At the time of this report, the only other known molecular structure for a six-coordinate iron(III) complex cation bearing a (PP)2
X
2 ligand set was [(o-C6F4(PMe2)2)2FeCl2][BF4] (Higgins et al., 1985 ▸; Higgins & Levason, 1985 ▸). This particular species was synthesized through metathesis of the original tetrachloridoferrate(III) anion with HBF4. The initial salt, [(o-C6F4(PMe2)2)2FeCl2][FeCl4], prepared via a nearly 1:1 stoichiometric reaction of iron(III) chloride with o-C6F4(PMe2)2, was not structurally characterized.
Our group is interested in the application of bisphosphanes as supporting ligands within iron-catalyzed cross-coupling reactions. Numerous literature protocols for iron-catalyzed cross-coupling methods involve use of bisphosphanes as substoichiometric additives in conjunction with iron(II) or iron(III) salts, promoting the formation of the active catalyst in situ. Methods development in our laboratory using the dppen ligand in conjunction with iron(III) chloride resulted in the formation of [(dppen)2FeCl2][FeCl4] (1) from reaction mixtures and its subsequent structural characterization. As reported herein, 1 was then independently prepared via the method of Chatt & Hayter (1961 ▸). While we have not observed this compound to exhibit catalytic effectiveness in cross-coupling, a literature search indicated that this ionic complex was first synthesized in the 1970s using the same reaction stoichiometry (Levason et al., 1975 ▸). This report lacked structural characterization of the complex, but its formulation as a complex salt was supported by magnetic susceptibility, Mössbauer, and IR absorption measurements. Upon confirming the structure of 1, we sought to examine an analogous species, [(dpbz)2FeCl2][FeCl4] (2), by taking advantage of the same steric substitution at phosphorus, but with a slightly varied backbone character (ortho-phenylene in place of the C2H2 of dppen). Such studies are important as they expand the coordination chemistry library of iron(III) complexes bearing bisphosphane ligands. In addition, 1 and 2 join only two other structurally characterized examples of coordinatively saturated iron(III) monocations with a (PP)2 X 2 ligand set that have been synthesized without using oxidative methods (Miller et al., 2002 ▸, Higgins & Levason, 1985 ▸).
Structural commentary
Both 1 and 2 are characterized as six-coordinate complex cations in which the iron(III) center is ligated by two bisphosphane ligands (dppen in 1, dpbz in 2) in a trans fashion (see Scheme). The two retained chlorido ligands are thus coordinated axially, and the displaced chlorido ligand results in generation of a single tetrachloridoferrate(III) anion in both cases. Compound 1 (Fig. 1 ▸) crystallizes in the centrosymmetric space group C2/c. The iron atom of the cation is located at a crystallographic inversion center, resulting in Cl—Fe—Cl and trans P—Fe—P angles of 180°. Deviation from ideal octahedral geometry is due to the 80.92 (2)° bite angles of the P—Fe—P chelate rings (Table 1 ▸). The Fe—P distances are considerably longer than those of the other structurally characterized iron(III) cations with a (PP)2 X 2 donor set (range 2.29–2.34 Å; Groom et al., 2016 ▸, see Database survey below), but with shorter Fe—Cl distances than those of the other reported X = Cl compounds (range 2.23–2.25 Å). The ethylene backbones of each dppen ligand in the cation of 1 are bent out of the equatorial plane by 24.86 (8)°. The tetrachloridoferrate(III) anion lies along a crystallographic twofold axis that includes the metal center. Phenyl group C3—C8 (and thus its symmetry equivalent, Fig. 1 ▸) is modeled as disordered over two positions [0.561 (6):0.439 (6)].
Figure 1.
Displacement ellipsoid plot of 1 drawn at the 50% probability level with hydrogen atoms omitted. The full cation of the title formula is generated by a crystallographic inversion center (1 − x, 1 − y, 1 − z) at atom Fe1. The full anion is generated by a crystallographic twofold axis (−x, y, 
− z), which includes atom Fe2. The symmetry-equivalent atoms of the dichloromethane solvent molecule are generated by a crystallographic twofold axis (1 − x, y, − z) that contains atom C27.
Table 1. Selected geometric parameters (Å, °) for 1 .
| Fe1—Cl1 | 2.2135 (6) | Fe1—P2 | 2.3738 (6) |
| Fe1—P1 | 2.3662 (6) | ||
| Cl1i—Fe1—Cl1 | 180.0 | Cl1—Fe1—P2i | 87.58 (2) |
| Cl1—Fe1—P1 | 92.38 (2) | Cl1—Fe1—P2 | 92.42 (2) |
| Cl1—Fe1—P1i | 87.62 (2) | P1—Fe1—P2 | 80.92 (2) |
| P1—Fe1—P1i | 180.0 | P2i—Fe1—P2 | 180.0 |
Symmetry code: (i) 
.
The asymmetric unit of 2 contains the cation, anion, and solvent molecule in general positions. The solvent molecule was modeled as disordered over three positions [0.740 (3):0.136 (3):0.124 (3)]. Despite the structural similarity of the backbone linkers and steric periphery of dppen and dpbz, the space group assignment and crystallographic symmetry of 2 contrasted from 1. Metrically, however, 1 and 2 are quite similar. The axial chlorido ligands within the cation of 2 are located at Fe—Cl distances very close to that found in the cation of 1 and the Cl—Fe—Cl and trans P—Fe—P angles are very nearly linear (Fig. 2 ▸, Table 2 ▸). Additionally, the bite angles in the cation of 2 as well as Fe—Cl distances and Cl—Fe—Cl angles of its tetrachloridoferrate(III) anion are very similar to those of 1. As observed for the ethylene backbones of the dppen ligands of 1, the ortho-phenylene backbones of the dpbz ligands in 2 are also canted out the equatorial plane by 21.9 (1) and 22.9 (1)°. The crystal of 2 studied was an inversion twin, whose component mass ratio refined to 0.76 (3):0.24 (3).
Figure 2.
Displacement ellipsoid plot of 2 drawn at the 50% probability level with hydrogen atoms omitted. Only the major component of disorder of the dichloromethane solvent molecule is shown.
Table 2. Selected geometric parameters (Å, °) for 2 .
| Fe1—Cl2 | 2.218 (2) | Fe1—P2 | 2.376 (2) |
| Fe1—Cl1 | 2.223 (2) | Fe1—P4 | 2.377 (2) |
| Fe1—P3 | 2.374 (2) | Fe1—P1 | 2.388 (2) |
| Cl2—Fe1—Cl1 | 179.87 (12) | P3—Fe1—P4 | 80.75 (8) |
| Cl2—Fe1—P3 | 87.69 (8) | P2—Fe1—P4 | 179.33 (10) |
| Cl1—Fe1—P3 | 92.26 (8) | Cl2—Fe1—P1 | 92.05 (8) |
| Cl2—Fe1—P2 | 92.82 (8) | Cl1—Fe1—P1 | 87.99 (7) |
| Cl1—Fe1—P2 | 87.30 (8) | P3—Fe1—P1 | 179.74 (10) |
| P3—Fe1—P2 | 98.58 (8) | P2—Fe1—P1 | 81.38 (8) |
| Cl2—Fe1—P4 | 87.23 (8) | P4—Fe1—P1 | 99.29 (8) |
| Cl1—Fe1—P4 | 92.65 (8) |
Both 1 and 2 are dichloromethane solvates under the common crystallization procedure used (see below). In 1, the solvent molecule is located along a crystallographic twofold axis that includes the carbon atom. Crystal desolvation is suspected, since its occupancy only refined to 0.592 (4). In contrast, 2 was found to possess full occupation of co-crystallized dichloromethane, modeled as disordered over three general positions [0.740 (3):0.136 (3):0.124 (3)].
Supramolecular features
There are no significant supramolecular features beyond a few very weak C—H⋯Cl and C—H⋯π interactions.
Database survey
Outside of 1 and 2 reported herein, there are eight examples of ionic iron(III) compounds bearing trans-coordinating bisphosphane ligands in an overall (PP)2 A 2 (A = formally monoanionic ligand) environment reported in the Cambridge Structural Database (CSD, Version 5.39, update No. 2, February 2018; Groom et al., 2016 ▸). The axial A ligands of the cations include two chlorido (CSD refcode DABCEO, Higgins et al., 1985 ▸; recode VOBHUP, Field et al., 1990 ▸; recode XAZZIH, Field et al., 2000 ▸; refcode BAJLAA, Miller et al., 2002 ▸), bromido and hydrido (refcode PABSUG; Evans et al., 1992 ▸), and chlorido and alkynyl (refcodes NAWMIJ, NAWMOP, NAWMUV; Hoffert et al., 2011 ▸). These structures include a variety of counter-anions: [FeCl4]−, [BF4]−, [BPh4]−, [Cl]−, [SO3CF3]−, and [B(3,5-CF3Ph)4]−. Only one of these examples, trans-[(o-C6F4(PMe2)2)2FeCl2][BF4], contains a bisphosphane ligand with an unsaturated backbone linker (Higgins et al., 1985 ▸). Just as in 1 and 2, the fluoro-substituted ortho-phenylene backbone of trans-[(o-C6F4(PMe2)2)2FeCl2][BF4] is also bent out of from the FeP4 equatorial plane (17.6 °).
Synthesis and crystallization
Anhydrous FeCl3 (98%, Alfa Aesar), cis-1,2-bis(diphenylphosphanel)ethylene (dppen, 98%, Strem), and 1,2-bis(diphenylphosphane)benzene (dpbz, 98%, Strem) were used in the synthesis of 1 and 2 without further purification. The syntheses of both compounds were performed under a dinitrogen atmosphere in a drybox. 80 mg FeCl3 (0.49 mmol) was dissolved in 5 ml THF (Aldrich, anhydrous, 99.9%, inhibitor-free), resulting in a yellow–green solution. In a separate vial, 200 mg dppen (or 225 mg dpbz for 2, 0.50 mmol in either case) was dissolved in 10 ml THF. At room temperature, the solution of bisphosphane was added to the stirring solution of FeCl3, resulting in immediate formation of a dark green precipitate in both cases. Each reaction was stirred for 5 min following complete addition of the bisphosphane solution, filtered, and the resulting green solid was dried under vacuum. In both cases, analytically pure microcrystalline solid was isolated in nearly quantitative yield. [FeCl2(dppen)2][FeCl4]: Yield: 94%. Elemental analysis: calculated: 55.903 C, 3.970 H; found: 56.327 C, 4.342 H. [FeCl2(dpbz)2][FeCl4]: Yield: 89%. Elemental analysis: calculated: 59.199 C, 3.974 H; found: 59.526 C, 4.452.
Once isolated and dried, solid 1 and 2 were found to be indefinitely stable outside of an inert atmosphere (greater than one year). Both complexes were crystallized by layering toluene over a concentrated dichloromethane solution of the complex and allowing the layers to diffuse at room temperature (anhydrous solvents were not used during crystallizations). Red–green dichroic single crystals suitable for X-ray diffraction studies were generally observed to crystallize within 24 h. Out of a large number of polar and non-polar common organic solvents examined, only dichloromethane, chloroform, acetone, and nitromethane appreciably solubilized 1 and 2. During preparation of crystallizations, dichloromethane solutions of 1 and 2 were observed under incandescent light to be green at low concentrations and red at high concentrations.
Refinement
Crystal data, data collection and structure refinement details are summarized in Table 3 ▸.
Table 3. Experimental details.
| 1 | 2 | |
|---|---|---|
| Crystal data | ||
| Chemical formula | [FeCl2(C26H22P2)2][FeCl4]·0.59CH2Cl2 | [FeCl2(C30H24P2)2][FeCl4]·CH2Cl2 |
| M r | 1167.47 | 1302.19 |
| Crystal system, space group | Monoclinic, C2/c | Triclinic, P1 |
| Temperature (K) | 100 | 100 |
| a, b, c (Å) | 9.7528 (7), 23.6871 (17), 23.6871 (17) | 9.8771 (7), 12.6516 (8), 12.8258 (8) |
| α, β, γ (°) | 90, 100.541 (2), 90 | 81.058 (1), 83.050 (1), 68.335 (1) |
| V (Å3) | 5379.7 (7) | 1467.87 (17) |
| Z | 4 | 1 |
| Radiation type | Mo Kα | Mo Kα |
| μ (mm−1) | 1.05 | 1.01 |
| Crystal size (mm) | 0.22 × 0.22 × 0.10 | 0.24 × 0.20 × 0.08 |
| Data collection | ||
| Diffractometer | Bruker SMART APEX II CCD platform | Bruker SMART APEX II CCD platform |
| Absorption correction | Multi-scan (SADABS; Krause et al., 2015 ▸) | Multi-scan (SADABS; Krause et al., 2015 ▸) |
| T min, T max | 0.643, 0.746 | 0.644, 0.747 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 71735, 8962, 6273 | 27211, 22268, 11890 |
| R int | 0.091 | 0.050 |
| (sin θ/λ)max (Å−1) | 0.736 | 0.807 |
| Refinement | ||
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.048, 0.119, 1.05 | 0.073, 0.182, 1.00 |
| No. of reflections | 8962 | 22268 |
| No. of parameters | 325 | 488 |
| No. of restraints | 33 | 34 |
| H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 0.74, −0.67 | 1.23, −1.39 |
| Absolute structure | – | Refined as an inversion twin. |
| Absolute structure parameter | – | 0.24 (3) |
Phenyl ring C3–C8 of 1 was modeled as disordered over two general positions [0.561 (6):0.439 (6)]. Analogous bond lengths and angles between the two positions and in both directions around the rings were restrained to be similar. Additionally the P1—C3 and P1—C3′ bond lengths were restrained to be similar. Anisotropic displacement parameters for pairs of proximal atoms were constrained to be equivalent. The occupancy of the cocrystallized dichloromethane solvent molecule refined to 0.592 (4), which is consistent with crystal desolvation.
2 was refined as an inversion twin in P1 whose twin component mass ratio refined to 0.76 (3):0.24 (3). Because of significant parameter correlation, anisotropic displacement parameters for pseudosymmetrically related atom pairs were constrained to be equivalent. The co-crystallized dichloromethane solvent molecule is modeled as disordered over three positions [0.740 (3):0.136 (3):0.124 (3)]. Analogous bond lengths and angles among the three positions of the disordered dichloromethane solvent molecule were restrained to be similar. Anisotropic displacement parameters for proximal and pseudosymmetrically related atoms were constrained to be equivalent.
A solution and refinement of 2 in centrosymmetric space group P
caused an increase in the R1 residual (strong data) from 0.071 to 0.118, which was not unexpected given the uneven twin component mass ratio when refined in P1. In the centrosymmetric model, the anion and solvent were modeled pairwise as disordered over a crystallographic inversion center.
H atoms were given riding models: aromatic/sp 2, C—H = 0.95 Å, and methylene, C—H = 0.99 Å, with U iso(H) = 1.2U eq(C).
For 1 the maximum residual peak of 0.74 e− Å−3 and the deepest hole of −0.67 e− Å−3 are found 0.72 and 0.82 Å, respectively, from atom CL4.
For 2 the maximum residual peak of 1.23 e− Å−3 and the deepest hole of −1.39 e− Å−3 are found 0.22 and 0.05 Å from atoms CL5 and C61 of the disordered solvent molcule, respectively.
Supplementary Material
Crystal structure: contains datablock(s) 1, 2, global. DOI: 10.1107/S2056989018006898/pj2052sup1.cif
Structure factors: contains datablock(s) 1. DOI: 10.1107/S2056989018006898/pj20521sup2.hkl
Structure factors: contains datablock(s) 2. DOI: 10.1107/S2056989018006898/pj20522sup3.hkl
Additional supporting information: crystallographic information; 3D view; checkCIF report
Acknowledgments
DM and DB thank the University of Rochester David T. Kearns Center for Leadership and Diversity and Professor Neidig for the opportunity to participate in this research. JLK thanks the Kearns Center as well as the University of Rochester Center for the Integration of Research, Teaching, and Learning for a research mentoring fellowship.
supplementary crystallographic information
trans-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane 0.59-solvate (1) . Crystal data
| [FeCl2(C26H22P2)2][FeCl4]·0.59CH2Cl2 | F(000) = 2380 |
| Mr = 1167.47 | Dx = 1.441 Mg m−3 |
| Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
| a = 9.7528 (7) Å | Cell parameters from 4040 reflections |
| b = 23.6871 (17) Å | θ = 2.3–29.5° |
| c = 23.6871 (17) Å | µ = 1.05 mm−1 |
| β = 100.541 (2)° | T = 100 K |
| V = 5379.7 (7) Å3 | Plate, red-violet |
| Z = 4 | 0.22 × 0.22 × 0.10 mm |
trans-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane 0.59-solvate (1) . Data collection
| Bruker SMART APEX II CCD platform diffractometer | 6273 reflections with I > 2σ(I) |
| Radiation source: fine-focus sealed tube | Rint = 0.091 |
| ω scans | θmax = 31.5°, θmin = 1.7° |
| Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −14→14 |
| Tmin = 0.643, Tmax = 0.746 | k = −34→34 |
| 71735 measured reflections | l = −34→34 |
| 8962 independent reflections |
trans-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane 0.59-solvate (1) . Refinement
| Refinement on F2 | Primary atom site location: dual |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| R[F2 > 2σ(F2)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.119 | H-atom parameters constrained |
| S = 1.05 | w = 1/[σ2(Fo2) + (0.0418P)2 + 11.3134P] where P = (Fo2 + 2Fc2)/3 |
| 8962 reflections | (Δ/σ)max = 0.001 |
| 325 parameters | Δρmax = 0.74 e Å−3 |
| 33 restraints | Δρmin = −0.67 e Å−3 |
trans-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane 0.59-solvate (1) . Special details
| 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. Phenyl ring C3-C8 is modeled as disordered over two positions (56:44). Analogous bond lengths and angles between the two positions were restrained to be similar. Anisotropic displacement parameters for pairs of proximal atoms were constrained to be equivalent. The occupancy of the cocrystallized dichloromethane solvent molecule refined to 0.592 (4). |
trans-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane 0.59-solvate (1) . Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Fe1 | 0.500000 | 0.500000 | 0.500000 | 0.01605 (10) | |
| Cl1 | 0.71798 (6) | 0.53023 (2) | 0.52215 (2) | 0.02045 (12) | |
| P1 | 0.46240 (6) | 0.51308 (3) | 0.59502 (3) | 0.01981 (13) | |
| P2 | 0.56127 (7) | 0.40841 (3) | 0.53686 (3) | 0.02134 (13) | |
| C1 | 0.4343 (3) | 0.44397 (12) | 0.62312 (12) | 0.0295 (6) | |
| H1 | 0.390120 | 0.440031 | 0.655474 | 0.035* | |
| C2 | 0.4761 (3) | 0.39907 (12) | 0.59802 (13) | 0.0321 (6) | |
| H2 | 0.461628 | 0.362302 | 0.611842 | 0.038* | |
| C3 | 0.605 (2) | 0.5342 (6) | 0.6520 (8) | 0.0227 (16) | 0.439 (6) |
| C4 | 0.6555 (15) | 0.4985 (4) | 0.6979 (5) | 0.0311 (15) | 0.439 (6) |
| H4 | 0.618358 | 0.461673 | 0.699969 | 0.037* | 0.439 (6) |
| C5 | 0.7618 (11) | 0.5184 (4) | 0.7406 (4) | 0.0393 (15) | 0.439 (6) |
| H5 | 0.798729 | 0.494642 | 0.772091 | 0.047* | 0.439 (6) |
| C6 | 0.8136 (10) | 0.5718 (4) | 0.7377 (4) | 0.0386 (16) | 0.439 (6) |
| H6 | 0.885234 | 0.584895 | 0.767556 | 0.046* | 0.439 (6) |
| C7 | 0.7637 (10) | 0.6067 (4) | 0.6925 (4) | 0.0322 (13) | 0.439 (6) |
| H7 | 0.801045 | 0.643578 | 0.690908 | 0.039* | 0.439 (6) |
| C8 | 0.6576 (15) | 0.5879 (5) | 0.6487 (6) | 0.0258 (14) | 0.439 (6) |
| H8 | 0.622193 | 0.611721 | 0.617137 | 0.031* | 0.439 (6) |
| C3' | 0.5987 (16) | 0.5479 (4) | 0.6468 (6) | 0.0227 (16) | 0.561 (6) |
| C4' | 0.6649 (11) | 0.5188 (3) | 0.6964 (4) | 0.0311 (15) | 0.561 (6) |
| H4' | 0.640148 | 0.480827 | 0.702639 | 0.037* | 0.561 (6) |
| C5' | 0.7671 (8) | 0.5460 (3) | 0.7365 (3) | 0.0393 (15) | 0.561 (6) |
| H5' | 0.810045 | 0.526376 | 0.770080 | 0.047* | 0.561 (6) |
| C6' | 0.8060 (7) | 0.6004 (3) | 0.7280 (3) | 0.0386 (16) | 0.561 (6) |
| H6' | 0.875271 | 0.618286 | 0.755653 | 0.046* | 0.561 (6) |
| C7' | 0.7444 (7) | 0.6293 (3) | 0.6793 (3) | 0.0322 (13) | 0.561 (6) |
| H7' | 0.771181 | 0.667151 | 0.673465 | 0.039* | 0.561 (6) |
| C8' | 0.6426 (11) | 0.6029 (3) | 0.6384 (4) | 0.0258 (14) | 0.561 (6) |
| H8' | 0.602754 | 0.622673 | 0.604511 | 0.031* | 0.561 (6) |
| C9 | 0.3051 (2) | 0.54964 (11) | 0.60637 (10) | 0.0213 (5) | |
| C10 | 0.3035 (3) | 0.60629 (12) | 0.62219 (12) | 0.0283 (5) | |
| H10 | 0.388476 | 0.626830 | 0.630628 | 0.034* | |
| C11 | 0.1786 (3) | 0.63282 (14) | 0.62566 (13) | 0.0377 (7) | |
| H11 | 0.177872 | 0.671691 | 0.635490 | 0.045* | |
| C12 | 0.0553 (3) | 0.60285 (15) | 0.61486 (13) | 0.0404 (8) | |
| H12 | −0.030285 | 0.621444 | 0.616380 | 0.048* | |
| C13 | 0.0553 (3) | 0.54595 (14) | 0.60185 (12) | 0.0338 (6) | |
| H13 | −0.029162 | 0.524979 | 0.596454 | 0.041* | |
| C14 | 0.1798 (2) | 0.51970 (12) | 0.59672 (11) | 0.0249 (5) | |
| H14 | 0.179670 | 0.480912 | 0.586525 | 0.030* | |
| C15 | 0.4992 (3) | 0.34577 (11) | 0.49472 (13) | 0.0292 (6) | |
| C16 | 0.3571 (3) | 0.33373 (12) | 0.48605 (16) | 0.0409 (8) | |
| H16 | 0.296816 | 0.356038 | 0.504190 | 0.049* | |
| C17 | 0.3039 (4) | 0.28904 (13) | 0.4508 (2) | 0.0542 (10) | |
| H17 | 0.206782 | 0.281126 | 0.444628 | 0.065* | |
| C18 | 0.3916 (4) | 0.25578 (13) | 0.4246 (2) | 0.0554 (10) | |
| H18 | 0.354057 | 0.226315 | 0.399149 | 0.066* | |
| C19 | 0.5340 (3) | 0.26585 (13) | 0.43563 (17) | 0.0434 (8) | |
| H19 | 0.594411 | 0.241985 | 0.419199 | 0.052* | |
| C20 | 0.5891 (3) | 0.31054 (11) | 0.47053 (13) | 0.0323 (6) | |
| H20 | 0.686832 | 0.317231 | 0.477997 | 0.039* | |
| C21 | 0.7448 (3) | 0.39546 (10) | 0.56642 (11) | 0.0235 (5) | |
| C22 | 0.8443 (3) | 0.40043 (10) | 0.53138 (11) | 0.0230 (5) | |
| H22 | 0.815723 | 0.409121 | 0.491821 | 0.028* | |
| C23 | 0.9851 (3) | 0.39282 (11) | 0.55371 (12) | 0.0270 (5) | |
| H23 | 1.052194 | 0.395727 | 0.529381 | 0.032* | |
| C24 | 1.0276 (3) | 0.38094 (11) | 0.61176 (13) | 0.0311 (6) | |
| H24 | 1.123860 | 0.376665 | 0.627434 | 0.037* | |
| C25 | 0.9290 (3) | 0.37537 (14) | 0.64658 (13) | 0.0383 (7) | |
| H25 | 0.957818 | 0.366739 | 0.686137 | 0.046* | |
| C26 | 0.7883 (3) | 0.38229 (13) | 0.62420 (12) | 0.0345 (6) | |
| H26 | 0.721343 | 0.378035 | 0.648409 | 0.041* | |
| Fe2 | 0.000000 | 0.80718 (2) | 0.750000 | 0.02335 (12) | |
| Cl2 | 0.18469 (8) | 0.86224 (3) | 0.76337 (3) | 0.03463 (16) | |
| Cl3 | −0.00845 (8) | 0.75564 (3) | 0.67250 (3) | 0.03743 (17) | |
| C27 | 0.500000 | 0.6989 (3) | 0.750000 | 0.055 (3) | 0.592 (4) |
| H27A | 0.480195 | 0.674166 | 0.781219 | 0.066* | 0.2960 (19) |
| H27B | 0.519802 | 0.674164 | 0.718782 | 0.066* | 0.2960 (19) |
| Cl4 | 0.35377 (18) | 0.73688 (9) | 0.72448 (9) | 0.0700 (8) | 0.592 (4) |
trans-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane 0.59-solvate (1) . Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Fe1 | 0.0147 (2) | 0.0175 (2) | 0.0161 (2) | −0.00051 (16) | 0.00312 (16) | −0.00011 (17) |
| Cl1 | 0.0159 (2) | 0.0237 (3) | 0.0217 (3) | −0.0022 (2) | 0.00337 (19) | −0.0017 (2) |
| P1 | 0.0166 (3) | 0.0264 (3) | 0.0167 (3) | 0.0014 (2) | 0.0037 (2) | 0.0001 (2) |
| P2 | 0.0204 (3) | 0.0198 (3) | 0.0252 (3) | 0.0025 (2) | 0.0079 (2) | 0.0039 (2) |
| C1 | 0.0302 (13) | 0.0347 (14) | 0.0263 (13) | 0.0083 (11) | 0.0126 (11) | 0.0114 (11) |
| C2 | 0.0319 (14) | 0.0316 (14) | 0.0368 (15) | 0.0083 (11) | 0.0173 (12) | 0.0163 (12) |
| C3 | 0.0173 (17) | 0.034 (5) | 0.016 (3) | 0.006 (4) | 0.0023 (13) | −0.002 (3) |
| C4 | 0.031 (2) | 0.040 (5) | 0.0219 (15) | 0.002 (4) | 0.0027 (14) | 0.000 (3) |
| C5 | 0.034 (2) | 0.058 (5) | 0.0226 (19) | 0.000 (4) | −0.0047 (16) | 0.002 (4) |
| C6 | 0.0271 (19) | 0.065 (5) | 0.023 (3) | −0.007 (4) | 0.0028 (18) | −0.012 (3) |
| C7 | 0.026 (2) | 0.046 (4) | 0.026 (3) | −0.011 (3) | 0.009 (2) | −0.011 (3) |
| C8 | 0.021 (2) | 0.036 (4) | 0.020 (3) | −0.002 (3) | 0.0026 (19) | −0.004 (3) |
| C3' | 0.0173 (17) | 0.034 (5) | 0.016 (3) | 0.006 (4) | 0.0023 (13) | −0.002 (3) |
| C4' | 0.031 (2) | 0.040 (5) | 0.0219 (15) | 0.002 (4) | 0.0027 (14) | 0.000 (3) |
| C5' | 0.034 (2) | 0.058 (5) | 0.0226 (19) | 0.000 (4) | −0.0047 (16) | 0.002 (4) |
| C6' | 0.0271 (19) | 0.065 (5) | 0.023 (3) | −0.007 (4) | 0.0028 (18) | −0.012 (3) |
| C7' | 0.026 (2) | 0.046 (4) | 0.026 (3) | −0.011 (3) | 0.009 (2) | −0.011 (3) |
| C8' | 0.021 (2) | 0.036 (4) | 0.020 (3) | −0.002 (3) | 0.0026 (19) | −0.004 (3) |
| C9 | 0.0175 (10) | 0.0288 (12) | 0.0181 (11) | 0.0019 (9) | 0.0044 (8) | −0.0001 (9) |
| C10 | 0.0304 (13) | 0.0308 (13) | 0.0259 (13) | 0.0005 (11) | 0.0108 (10) | −0.0028 (11) |
| C11 | 0.0471 (18) | 0.0383 (16) | 0.0328 (16) | 0.0147 (14) | 0.0204 (13) | 0.0000 (12) |
| C12 | 0.0314 (15) | 0.060 (2) | 0.0336 (16) | 0.0217 (14) | 0.0166 (12) | 0.0098 (15) |
| C13 | 0.0194 (12) | 0.0573 (19) | 0.0249 (13) | 0.0028 (12) | 0.0049 (10) | 0.0055 (13) |
| C14 | 0.0197 (11) | 0.0357 (14) | 0.0200 (12) | −0.0018 (10) | 0.0056 (9) | −0.0004 (10) |
| C15 | 0.0264 (12) | 0.0180 (11) | 0.0436 (16) | 0.0006 (10) | 0.0076 (11) | 0.0021 (11) |
| C16 | 0.0257 (13) | 0.0199 (13) | 0.079 (2) | −0.0008 (11) | 0.0139 (15) | 0.0006 (14) |
| C17 | 0.0311 (16) | 0.0241 (15) | 0.106 (3) | −0.0062 (12) | 0.0070 (18) | −0.0078 (18) |
| C18 | 0.0420 (18) | 0.0233 (15) | 0.097 (3) | −0.0058 (13) | 0.0033 (19) | −0.0179 (17) |
| C19 | 0.0376 (16) | 0.0255 (14) | 0.067 (2) | 0.0009 (12) | 0.0100 (16) | −0.0107 (14) |
| C20 | 0.0289 (13) | 0.0230 (13) | 0.0455 (17) | 0.0009 (10) | 0.0083 (12) | −0.0008 (12) |
| C21 | 0.0243 (11) | 0.0218 (11) | 0.0245 (12) | 0.0052 (9) | 0.0049 (9) | 0.0028 (9) |
| C22 | 0.0231 (11) | 0.0226 (11) | 0.0227 (12) | 0.0022 (9) | 0.0023 (9) | 0.0021 (9) |
| C23 | 0.0221 (11) | 0.0265 (13) | 0.0319 (14) | 0.0030 (10) | 0.0034 (10) | 0.0004 (10) |
| C24 | 0.0271 (13) | 0.0269 (13) | 0.0364 (15) | 0.0047 (10) | −0.0022 (11) | −0.0031 (11) |
| C25 | 0.0423 (17) | 0.0458 (18) | 0.0245 (14) | 0.0140 (14) | −0.0001 (12) | 0.0050 (12) |
| C26 | 0.0362 (15) | 0.0416 (16) | 0.0270 (14) | 0.0135 (13) | 0.0091 (12) | 0.0083 (12) |
| Fe2 | 0.0267 (3) | 0.0208 (2) | 0.0222 (3) | 0.000 | 0.0037 (2) | 0.000 |
| Cl2 | 0.0376 (4) | 0.0405 (4) | 0.0270 (3) | −0.0135 (3) | 0.0093 (3) | −0.0080 (3) |
| Cl3 | 0.0409 (4) | 0.0326 (4) | 0.0387 (4) | −0.0027 (3) | 0.0071 (3) | −0.0155 (3) |
| C27 | 0.026 (4) | 0.030 (4) | 0.101 (8) | 0.000 | −0.010 (4) | 0.000 |
| Cl4 | 0.0446 (9) | 0.0845 (14) | 0.0813 (14) | 0.0320 (9) | 0.0126 (8) | 0.0329 (10) |
trans-Bis[1,2-bis(diphenylphosphane)ethylene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane 0.59-solvate (1) . Geometric parameters (Å, º)
| Fe1—Cl1i | 2.2135 (6) | C10—C11 | 1.387 (4) |
| Fe1—Cl1 | 2.2135 (6) | C10—H10 | 0.9500 |
| Fe1—P1 | 2.3662 (6) | C11—C12 | 1.379 (5) |
| Fe1—P1i | 2.3662 (6) | C11—H11 | 0.9500 |
| Fe1—P2i | 2.3738 (6) | C12—C13 | 1.383 (5) |
| Fe1—P2 | 2.3738 (6) | C12—H12 | 0.9500 |
| P1—C1 | 1.807 (3) | C13—C14 | 1.390 (4) |
| P1—C3 | 1.822 (6) | C13—H13 | 0.9500 |
| P1—C9 | 1.824 (2) | C14—H14 | 0.9500 |
| P1—C3' | 1.832 (5) | C15—C16 | 1.393 (4) |
| P2—C2 | 1.811 (3) | C15—C20 | 1.406 (4) |
| P2—C21 | 1.825 (3) | C16—C17 | 1.388 (5) |
| P2—C15 | 1.829 (3) | C16—H16 | 0.9500 |
| C1—C2 | 1.319 (4) | C17—C18 | 1.391 (5) |
| C1—H1 | 0.9500 | C17—H17 | 0.9500 |
| C2—H2 | 0.9500 | C18—C19 | 1.386 (5) |
| C3—C8 | 1.379 (10) | C18—H18 | 0.9500 |
| C3—C4 | 1.393 (10) | C19—C20 | 1.389 (4) |
| C4—C5 | 1.391 (10) | C19—H19 | 0.9500 |
| C4—H4 | 0.9500 | C20—H20 | 0.9500 |
| C5—C6 | 1.369 (10) | C21—C26 | 1.392 (4) |
| C5—H5 | 0.9500 | C21—C22 | 1.393 (4) |
| C6—C7 | 1.370 (10) | C22—C23 | 1.390 (3) |
| C6—H6 | 0.9500 | C22—H22 | 0.9500 |
| C7—C8 | 1.397 (10) | C23—C24 | 1.390 (4) |
| C7—H7 | 0.9500 | C23—H23 | 0.9500 |
| C8—H8 | 0.9500 | C24—C25 | 1.383 (4) |
| C3'—C8' | 1.396 (8) | C24—H24 | 0.9500 |
| C3'—C4' | 1.413 (8) | C25—C26 | 1.387 (4) |
| C4'—C5' | 1.401 (8) | C25—H25 | 0.9500 |
| C4'—H4' | 0.9500 | C26—H26 | 0.9500 |
| C5'—C6' | 1.368 (8) | Fe2—Cl3ii | 2.1936 (8) |
| C5'—H5' | 0.9500 | Fe2—Cl3 | 2.1937 (8) |
| C6'—C7' | 1.382 (8) | Fe2—Cl2 | 2.1993 (8) |
| C6'—H6' | 0.9500 | Fe2—Cl2ii | 2.1993 (7) |
| C7'—C8' | 1.401 (8) | C27—Cl4iii | 1.701 (4) |
| C7'—H7' | 0.9500 | C27—Cl4 | 1.701 (4) |
| C8'—H8' | 0.9500 | C27—H27A | 0.9900 |
| C9—C10 | 1.394 (4) | C27—H27B | 0.9900 |
| C9—C14 | 1.395 (3) | ||
| Cl1i—Fe1—Cl1 | 180.0 | C3'—C8'—C7' | 121.0 (6) |
| Cl1i—Fe1—P1 | 87.63 (2) | C3'—C8'—H8' | 119.5 |
| Cl1—Fe1—P1 | 92.38 (2) | C7'—C8'—H8' | 119.5 |
| Cl1i—Fe1—P1i | 92.38 (2) | C10—C9—C14 | 118.8 (2) |
| Cl1—Fe1—P1i | 87.62 (2) | C10—C9—P1 | 123.18 (19) |
| P1—Fe1—P1i | 180.0 | C14—C9—P1 | 118.00 (19) |
| Cl1i—Fe1—P2i | 92.42 (2) | C11—C10—C9 | 120.3 (3) |
| Cl1—Fe1—P2i | 87.58 (2) | C11—C10—H10 | 119.8 |
| P1—Fe1—P2i | 99.08 (2) | C9—C10—H10 | 119.8 |
| P1i—Fe1—P2i | 80.92 (2) | C12—C11—C10 | 120.1 (3) |
| Cl1i—Fe1—P2 | 87.58 (2) | C12—C11—H11 | 120.0 |
| Cl1—Fe1—P2 | 92.42 (2) | C10—C11—H11 | 120.0 |
| P1—Fe1—P2 | 80.92 (2) | C11—C12—C13 | 120.5 (3) |
| P1i—Fe1—P2 | 99.08 (2) | C11—C12—H12 | 119.7 |
| P2i—Fe1—P2 | 180.0 | C13—C12—H12 | 119.7 |
| C1—P1—C3 | 97.0 (4) | C12—C13—C14 | 119.4 (3) |
| C1—P1—C9 | 100.81 (12) | C12—C13—H13 | 120.3 |
| C3—P1—C9 | 108.1 (9) | C14—C13—H13 | 120.3 |
| C1—P1—C3' | 107.6 (3) | C13—C14—C9 | 120.8 (3) |
| C9—P1—C3' | 102.4 (7) | C13—C14—H14 | 119.6 |
| C1—P1—Fe1 | 106.98 (9) | C9—C14—H14 | 119.6 |
| C3—P1—Fe1 | 120.7 (9) | C16—C15—C20 | 119.8 (3) |
| C9—P1—Fe1 | 118.90 (8) | C16—C15—P2 | 117.9 (2) |
| C3'—P1—Fe1 | 118.4 (7) | C20—C15—P2 | 122.4 (2) |
| C2—P2—C21 | 103.54 (13) | C17—C16—C15 | 119.8 (3) |
| C2—P2—C15 | 100.56 (14) | C17—C16—H16 | 120.1 |
| C21—P2—C15 | 106.04 (12) | C15—C16—H16 | 120.1 |
| C2—P2—Fe1 | 106.53 (9) | C16—C17—C18 | 120.5 (3) |
| C21—P2—Fe1 | 117.26 (9) | C16—C17—H17 | 119.7 |
| C15—P2—Fe1 | 120.33 (9) | C18—C17—H17 | 119.7 |
| C2—C1—P1 | 119.0 (2) | C19—C18—C17 | 119.6 (3) |
| C2—C1—H1 | 120.5 | C19—C18—H18 | 120.2 |
| P1—C1—H1 | 120.5 | C17—C18—H18 | 120.2 |
| C1—C2—P2 | 119.1 (2) | C18—C19—C20 | 120.6 (3) |
| C1—C2—H2 | 120.4 | C18—C19—H19 | 119.7 |
| P2—C2—H2 | 120.4 | C20—C19—H19 | 119.7 |
| C8—C3—C4 | 121.4 (7) | C19—C20—C15 | 119.5 (3) |
| C8—C3—P1 | 116.9 (8) | C19—C20—H20 | 120.3 |
| C4—C3—P1 | 121.7 (8) | C15—C20—H20 | 120.3 |
| C5—C4—C3 | 118.2 (8) | C26—C21—C22 | 119.0 (2) |
| C5—C4—H4 | 120.9 | C26—C21—P2 | 121.0 (2) |
| C3—C4—H4 | 120.9 | C22—C21—P2 | 119.92 (19) |
| C6—C5—C4 | 120.6 (8) | C23—C22—C21 | 120.6 (2) |
| C6—C5—H5 | 119.7 | C23—C22—H22 | 119.7 |
| C4—C5—H5 | 119.7 | C21—C22—H22 | 119.7 |
| C5—C6—C7 | 121.0 (8) | C22—C23—C24 | 119.8 (3) |
| C5—C6—H6 | 119.5 | C22—C23—H23 | 120.1 |
| C7—C6—H6 | 119.5 | C24—C23—H23 | 120.1 |
| C6—C7—C8 | 119.8 (8) | C25—C24—C23 | 119.7 (3) |
| C6—C7—H7 | 120.1 | C25—C24—H24 | 120.1 |
| C8—C7—H7 | 120.1 | C23—C24—H24 | 120.1 |
| C3—C8—C7 | 119.0 (8) | C24—C25—C26 | 120.5 (3) |
| C3—C8—H8 | 120.5 | C24—C25—H25 | 119.7 |
| C7—C8—H8 | 120.5 | C26—C25—H25 | 119.7 |
| C8'—C3'—C4' | 117.9 (5) | C25—C26—C21 | 120.3 (3) |
| C8'—C3'—P1 | 121.9 (6) | C25—C26—H26 | 119.9 |
| C4'—C3'—P1 | 120.2 (6) | C21—C26—H26 | 119.9 |
| C5'—C4'—C3' | 119.9 (6) | Cl3ii—Fe2—Cl3 | 112.36 (5) |
| C5'—C4'—H4' | 120.0 | Cl3ii—Fe2—Cl2 | 107.77 (3) |
| C3'—C4'—H4' | 120.0 | Cl3—Fe2—Cl2 | 110.79 (3) |
| C6'—C5'—C4' | 121.0 (6) | Cl3ii—Fe2—Cl2ii | 110.79 (3) |
| C6'—C5'—H5' | 119.5 | Cl3—Fe2—Cl2ii | 107.76 (3) |
| C4'—C5'—H5' | 119.5 | Cl2—Fe2—Cl2ii | 107.26 (5) |
| C5'—C6'—C7' | 120.0 (6) | Cl4iii—C27—Cl4 | 116.2 (5) |
| C5'—C6'—H6' | 120.0 | Cl4iii—C27—H27A | 108.2 |
| C7'—C6'—H6' | 120.0 | Cl4—C27—H27A | 108.2 |
| C6'—C7'—C8' | 120.0 (6) | Cl4iii—C27—H27B | 108.2 |
| C6'—C7'—H7' | 120.0 | Cl4—C27—H27B | 108.2 |
| C8'—C7'—H7' | 120.0 | H27A—C27—H27B | 107.4 |
| C3—P1—C1—C2 | −105.9 (10) | C1—P1—C9—C14 | −38.8 (2) |
| C9—P1—C1—C2 | 144.1 (2) | C3—P1—C9—C14 | −140.0 (5) |
| C3'—P1—C1—C2 | −109.1 (8) | C3'—P1—C9—C14 | −149.7 (4) |
| Fe1—P1—C1—C2 | 19.1 (3) | Fe1—P1—C9—C14 | 77.6 (2) |
| P1—C1—C2—P2 | 0.6 (4) | C14—C9—C10—C11 | −2.9 (4) |
| C21—P2—C2—C1 | 104.4 (3) | P1—C9—C10—C11 | 174.8 (2) |
| C15—P2—C2—C1 | −146.1 (3) | C9—C10—C11—C12 | 1.6 (4) |
| Fe1—P2—C2—C1 | −19.9 (3) | C10—C11—C12—C13 | 1.5 (5) |
| C1—P1—C3—C8 | −177 (2) | C11—C12—C13—C14 | −3.4 (4) |
| C9—P1—C3—C8 | −74 (2) | C12—C13—C14—C9 | 2.1 (4) |
| Fe1—P1—C3—C8 | 68 (2) | C10—C9—C14—C13 | 1.0 (4) |
| C1—P1—C3—C4 | 0 (2) | P1—C9—C14—C13 | −176.8 (2) |
| C9—P1—C3—C4 | 104 (2) | C2—P2—C15—C16 | 47.9 (3) |
| Fe1—P1—C3—C4 | −114 (2) | C21—P2—C15—C16 | 155.4 (2) |
| C8—C3—C4—C5 | 0 (4) | Fe1—P2—C15—C16 | −68.5 (3) |
| P1—C3—C4—C5 | −178.0 (16) | C2—P2—C15—C20 | −133.1 (3) |
| C3—C4—C5—C6 | 1 (2) | C21—P2—C15—C20 | −25.5 (3) |
| C4—C5—C6—C7 | −0.9 (19) | Fe1—P2—C15—C20 | 110.6 (2) |
| C5—C6—C7—C8 | 0.5 (18) | C20—C15—C16—C17 | −3.8 (5) |
| C4—C3—C8—C7 | 0 (4) | P2—C15—C16—C17 | 175.2 (3) |
| P1—C3—C8—C7 | 177.7 (14) | C15—C16—C17—C18 | 0.7 (6) |
| C6—C7—C8—C3 | 0 (3) | C16—C17—C18—C19 | 2.8 (6) |
| C1—P1—C3'—C8' | −178.4 (15) | C17—C18—C19—C20 | −3.1 (6) |
| C9—P1—C3'—C8' | −72.6 (18) | C18—C19—C20—C15 | 0.0 (5) |
| Fe1—P1—C3'—C8' | 60.3 (18) | C16—C15—C20—C19 | 3.5 (5) |
| C1—P1—C3'—C4' | 2.9 (18) | P2—C15—C20—C19 | −175.5 (3) |
| C9—P1—C3'—C4' | 108.6 (15) | C2—P2—C21—C26 | −0.4 (3) |
| Fe1—P1—C3'—C4' | −118.4 (14) | C15—P2—C21—C26 | −105.7 (2) |
| C8'—C3'—C4'—C5' | 3 (2) | Fe1—P2—C21—C26 | 116.6 (2) |
| P1—C3'—C4'—C5' | −178.7 (11) | C2—P2—C21—C22 | −178.3 (2) |
| C3'—C4'—C5'—C6' | −1.0 (18) | C15—P2—C21—C22 | 76.3 (2) |
| C4'—C5'—C6'—C7' | −0.2 (13) | Fe1—P2—C21—C22 | −61.4 (2) |
| C5'—C6'—C7'—C8' | −0.2 (13) | C26—C21—C22—C23 | −0.5 (4) |
| C4'—C3'—C8'—C7' | −3 (3) | P2—C21—C22—C23 | 177.5 (2) |
| P1—C3'—C8'—C7' | 178.3 (11) | C21—C22—C23—C24 | −1.0 (4) |
| C6'—C7'—C8'—C3' | 1.8 (19) | C22—C23—C24—C25 | 1.6 (4) |
| C1—P1—C9—C10 | 143.5 (2) | C23—C24—C25—C26 | −0.9 (5) |
| C3—P1—C9—C10 | 42.3 (6) | C24—C25—C26—C21 | −0.6 (5) |
| C3'—P1—C9—C10 | 32.6 (5) | C22—C21—C26—C25 | 1.2 (4) |
| Fe1—P1—C9—C10 | −100.1 (2) | P2—C21—C26—C25 | −176.7 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, y, −z+3/2; (iii) −x+1, y, −z+3/2.
trans-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane monosolvate (2) . Crystal data
| [FeCl2(C30H24P2)2][FeCl4]·CH2Cl2 | Z = 1 |
| Mr = 1302.19 | F(000) = 664 |
| Triclinic, P1 | Dx = 1.473 Mg m−3 |
| a = 9.8771 (7) Å | Mo Kα radiation, λ = 0.71073 Å |
| b = 12.6516 (8) Å | Cell parameters from 4051 reflections |
| c = 12.8258 (8) Å | θ = 2.3–30.7° |
| α = 81.058 (1)° | µ = 1.01 mm−1 |
| β = 83.050 (1)° | T = 100 K |
| γ = 68.335 (1)° | Plate, dichroic red-green |
| V = 1467.87 (17) Å3 | 0.24 × 0.20 × 0.08 mm |
trans-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane monosolvate (2) . Data collection
| Bruker SMART APEX II CCD platform diffractometer | 11890 reflections with I > 2σ(I) |
| Radiation source: fine-focus sealed tube | Rint = 0.050 |
| ω scans | θmax = 35.0°, θmin = 2.2° |
| Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −15→15 |
| Tmin = 0.644, Tmax = 0.747 | k = −20→20 |
| 27211 measured reflections | l = −20→18 |
| 22268 independent reflections |
trans-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane monosolvate (2) . Refinement
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.073 | H-atom parameters constrained |
| wR(F2) = 0.182 | w = 1/[σ2(Fo2) + (0.0641P)2] where P = (Fo2 + 2Fc2)/3 |
| S = 1.00 | (Δ/σ)max < 0.001 |
| 22268 reflections | Δρmax = 1.23 e Å−3 |
| 488 parameters | Δρmin = −1.39 e Å−3 |
| 34 restraints | Absolute structure: Refined as an inversion twin. |
| Primary atom site location: dual | Absolute structure parameter: 0.24 (3) |
trans-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane monosolvate (2) . Special details
| 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. The structure was modeled as an inversion twin whose component mass ratio refined to 0.76 (3):0.24 (3). A solution and refinement in centrosymmetric space group P-1 caused an increase in the R1 residual (strong data) from 0.071 to 0.118. The cocrystallized dichloromethane solvent molecule is modeled as disordered over three positions (0.740 (3):0.136 (3):0.124 (3)). Analogous bond lengths and angles among the three positions of the disordered dichloromethane solvent molecule were restrained to be similar. Anisotropic displacement parameters for proximal and pseudosymmetrically related atoms were constrained to be equivalent. |
trans-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane monosolvate (2) . Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Fe1 | 0.50286 (14) | 0.39706 (10) | 0.63842 (10) | 0.01341 (15) | |
| Cl1 | 0.68914 (19) | 0.42220 (14) | 0.69888 (14) | 0.01712 (17) | |
| Cl2 | 0.31700 (19) | 0.37173 (15) | 0.57842 (14) | 0.01712 (17) | |
| P1 | 0.3591 (2) | 0.59048 (15) | 0.66544 (16) | 0.01471 (18) | |
| P2 | 0.5609 (2) | 0.48921 (15) | 0.47244 (15) | 0.01494 (19) | |
| P3 | 0.6449 (2) | 0.20476 (15) | 0.61113 (16) | 0.01471 (18) | |
| P4 | 0.4468 (2) | 0.30281 (15) | 0.80391 (15) | 0.01494 (19) | |
| C1 | 0.4350 (8) | 0.6828 (6) | 0.5755 (6) | 0.0168 (7) | |
| C2 | 0.4012 (9) | 0.7982 (6) | 0.5880 (7) | 0.0203 (8) | |
| H2 | 0.342059 | 0.829432 | 0.647917 | 0.024* | |
| C3 | 0.4557 (9) | 0.8671 (7) | 0.5111 (7) | 0.0224 (8) | |
| H3 | 0.430915 | 0.945688 | 0.518605 | 0.027* | |
| C4 | 0.5440 (10) | 0.8228 (7) | 0.4253 (7) | 0.0230 (8) | |
| H4 | 0.580837 | 0.870627 | 0.374680 | 0.028* | |
| C5 | 0.5801 (10) | 0.7077 (7) | 0.4120 (7) | 0.0231 (8) | |
| H5 | 0.641033 | 0.677084 | 0.352542 | 0.028* | |
| C6 | 0.5258 (9) | 0.6381 (6) | 0.4871 (6) | 0.0168 (7) | |
| C7 | 0.3577 (9) | 0.6416 (6) | 0.7913 (6) | 0.0170 (7) | |
| C8 | 0.4891 (9) | 0.6487 (6) | 0.8184 (7) | 0.0185 (7) | |
| H8 | 0.573481 | 0.629636 | 0.770516 | 0.022* | |
| C9 | 0.4942 (10) | 0.6834 (7) | 0.9141 (7) | 0.0216 (8) | |
| H9 | 0.582948 | 0.686509 | 0.932254 | 0.026* | |
| C10 | 0.3734 (10) | 0.7134 (7) | 0.9833 (7) | 0.0253 (9) | |
| H10 | 0.378826 | 0.736978 | 1.049025 | 0.030* | |
| C11 | 0.2439 (10) | 0.7094 (7) | 0.9579 (7) | 0.0276 (10) | |
| H11 | 0.159982 | 0.730938 | 1.005926 | 0.033* | |
| C12 | 0.2351 (9) | 0.6736 (7) | 0.8613 (7) | 0.0217 (8) | |
| H12 | 0.145437 | 0.671463 | 0.843936 | 0.026* | |
| C13 | 0.1675 (9) | 0.6443 (7) | 0.6345 (7) | 0.0205 (8) | |
| C14 | 0.0746 (9) | 0.5937 (7) | 0.6896 (7) | 0.0234 (8) | |
| H14 | 0.110682 | 0.531331 | 0.743055 | 0.028* | |
| C15 | −0.0721 (10) | 0.6326 (8) | 0.6681 (8) | 0.0292 (10) | |
| H15 | −0.134976 | 0.597322 | 0.707755 | 0.035* | |
| C16 | −0.1257 (10) | 0.7200 (8) | 0.5913 (8) | 0.0308 (10) | |
| H16 | −0.225523 | 0.745221 | 0.576744 | 0.037* | |
| C17 | −0.0333 (11) | 0.7737 (8) | 0.5330 (8) | 0.0358 (11) | |
| H17 | −0.069872 | 0.834910 | 0.478609 | 0.043* | |
| C18 | 0.1131 (10) | 0.7356 (7) | 0.5564 (7) | 0.0272 (9) | |
| H18 | 0.175868 | 0.772242 | 0.518776 | 0.033* | |
| C19 | 0.4506 (8) | 0.5019 (6) | 0.3642 (6) | 0.0165 (7) | |
| C20 | 0.3450 (9) | 0.6064 (7) | 0.3297 (7) | 0.0254 (9) | |
| H20 | 0.333632 | 0.672703 | 0.361033 | 0.030* | |
| C21 | 0.2576 (10) | 0.6151 (8) | 0.2516 (7) | 0.0292 (10) | |
| H21 | 0.184693 | 0.686828 | 0.230899 | 0.035* | |
| C22 | 0.2737 (10) | 0.5204 (8) | 0.2020 (7) | 0.0262 (10) | |
| H22 | 0.215100 | 0.527670 | 0.145873 | 0.031* | |
| C23 | 0.3766 (9) | 0.4155 (7) | 0.2358 (6) | 0.0206 (9) | |
| H23 | 0.389282 | 0.349815 | 0.202910 | 0.025* | |
| C24 | 0.4610 (9) | 0.4065 (7) | 0.3178 (6) | 0.0187 (8) | |
| H24 | 0.527743 | 0.333368 | 0.342963 | 0.022* | |
| C25 | 0.7486 (9) | 0.4461 (7) | 0.4165 (6) | 0.0177 (7) | |
| C26 | 0.7991 (9) | 0.3814 (7) | 0.3313 (7) | 0.0246 (9) | |
| H26 | 0.732100 | 0.362996 | 0.296982 | 0.030* | |
| C27 | 0.9467 (10) | 0.3436 (9) | 0.2961 (8) | 0.0345 (11) | |
| H27 | 0.981402 | 0.297850 | 0.239587 | 0.041* | |
| C28 | 1.0437 (10) | 0.3753 (9) | 0.3469 (8) | 0.0346 (12) | |
| H28 | 1.144813 | 0.348675 | 0.324980 | 0.041* | |
| C29 | 0.9948 (10) | 0.4427 (8) | 0.4259 (8) | 0.0303 (11) | |
| H29 | 1.060584 | 0.465935 | 0.456527 | 0.036* | |
| C30 | 0.8479 (9) | 0.4781 (7) | 0.4623 (7) | 0.0228 (8) | |
| H30 | 0.814661 | 0.524277 | 0.518586 | 0.027* | |
| C31 | 0.5655 (8) | 0.1115 (6) | 0.7002 (6) | 0.0168 (7) | |
| C32 | 0.6008 (9) | −0.0039 (7) | 0.6850 (7) | 0.0203 (8) | |
| H32 | 0.661938 | −0.033872 | 0.625422 | 0.024* | |
| C33 | 0.5457 (9) | −0.0727 (7) | 0.7576 (7) | 0.0224 (8) | |
| H33 | 0.568623 | −0.150634 | 0.748200 | 0.027* | |
| C34 | 0.4560 (10) | −0.0278 (7) | 0.8449 (7) | 0.0230 (8) | |
| H34 | 0.417449 | −0.075317 | 0.894485 | 0.028* | |
| C35 | 0.4230 (10) | 0.0844 (7) | 0.8600 (7) | 0.0231 (8) | |
| H35 | 0.363418 | 0.113538 | 0.920434 | 0.028* | |
| C36 | 0.4772 (9) | 0.1564 (6) | 0.7861 (6) | 0.0168 (7) | |
| C37 | 0.6454 (9) | 0.1559 (6) | 0.4842 (6) | 0.0170 (7) | |
| C38 | 0.5193 (9) | 0.1451 (6) | 0.4567 (7) | 0.0185 (7) | |
| H38 | 0.435397 | 0.161863 | 0.505053 | 0.022* | |
| C39 | 0.5133 (10) | 0.1107 (7) | 0.3611 (7) | 0.0216 (8) | |
| H39 | 0.426161 | 0.104035 | 0.343895 | 0.026* | |
| C40 | 0.6362 (10) | 0.0858 (7) | 0.2894 (7) | 0.0253 (9) | |
| H40 | 0.632232 | 0.063705 | 0.222680 | 0.030* | |
| C41 | 0.7640 (10) | 0.0934 (7) | 0.3162 (7) | 0.0276 (10) | |
| H41 | 0.848092 | 0.075253 | 0.268098 | 0.033* | |
| C42 | 0.7695 (9) | 0.1273 (7) | 0.4130 (7) | 0.0217 (8) | |
| H42 | 0.857814 | 0.131138 | 0.431233 | 0.026* | |
| C43 | 0.8368 (9) | 0.1487 (7) | 0.6415 (7) | 0.0205 (8) | |
| C44 | 0.9319 (9) | 0.2031 (7) | 0.5899 (7) | 0.0234 (8) | |
| H44 | 0.894856 | 0.268358 | 0.539493 | 0.028* | |
| C45 | 1.0755 (10) | 0.1651 (8) | 0.6101 (8) | 0.0292 (10) | |
| H45 | 1.138383 | 0.201914 | 0.572957 | 0.035* | |
| C46 | 1.1292 (10) | 0.0697 (8) | 0.6873 (8) | 0.0308 (10) | |
| H46 | 1.228576 | 0.042808 | 0.703517 | 0.037* | |
| C47 | 1.0388 (11) | 0.0167 (8) | 0.7381 (8) | 0.0358 (11) | |
| H47 | 1.076749 | −0.048303 | 0.788638 | 0.043* | |
| C48 | 0.8941 (10) | 0.0544 (7) | 0.7185 (7) | 0.0272 (9) | |
| H48 | 0.832507 | 0.016987 | 0.756782 | 0.033* | |
| C49 | 0.5653 (8) | 0.2851 (6) | 0.9099 (6) | 0.0165 (7) | |
| C50 | 0.6609 (10) | 0.1782 (7) | 0.9469 (7) | 0.0254 (9) | |
| H50 | 0.664284 | 0.112121 | 0.918717 | 0.030* | |
| C51 | 0.7527 (10) | 0.1675 (8) | 1.0259 (7) | 0.0292 (10) | |
| H51 | 0.819167 | 0.094181 | 1.050727 | 0.035* | |
| C52 | 0.7467 (10) | 0.2646 (8) | 1.0683 (7) | 0.0262 (10) | |
| H52 | 0.809821 | 0.257491 | 1.121332 | 0.031* | |
| C53 | 0.6490 (9) | 0.3706 (7) | 1.0329 (6) | 0.0206 (9) | |
| H53 | 0.642575 | 0.436063 | 1.063628 | 0.025* | |
| C54 | 0.5595 (9) | 0.3826 (7) | 0.9523 (6) | 0.0187 (8) | |
| H54 | 0.495090 | 0.456324 | 0.926328 | 0.022* | |
| C55 | 0.2583 (9) | 0.3503 (7) | 0.8622 (6) | 0.0177 (7) | |
| C56 | 0.2117 (9) | 0.4183 (7) | 0.9441 (7) | 0.0246 (9) | |
| H56 | 0.280279 | 0.438387 | 0.974875 | 0.030* | |
| C57 | 0.0671 (10) | 0.4570 (9) | 0.9813 (8) | 0.0345 (11) | |
| H57 | 0.037337 | 0.503542 | 1.037323 | 0.041* | |
| C58 | −0.0343 (10) | 0.4296 (8) | 0.9388 (8) | 0.0346 (12) | |
| H58 | −0.134230 | 0.458287 | 0.963586 | 0.041* | |
| C59 | 0.0112 (10) | 0.3588 (8) | 0.8584 (8) | 0.0303 (11) | |
| H59 | −0.057673 | 0.337013 | 0.829994 | 0.036* | |
| C60 | 0.1560 (9) | 0.3200 (7) | 0.8196 (7) | 0.0228 (8) | |
| H60 | 0.185630 | 0.272858 | 0.764084 | 0.027* | |
| Fe2 | 0.74909 (13) | 0.79207 (11) | 0.09572 (11) | 0.0302 (3) | |
| Cl3 | 0.5310 (2) | 0.92270 (18) | 0.11580 (17) | 0.0339 (4) | |
| Cl4 | 0.7333 (3) | 0.62264 (18) | 0.13622 (18) | 0.0437 (6) | |
| Cl5 | 0.8376 (3) | 0.8101 (3) | −0.0681 (3) | 0.0645 (6) | |
| Cl6 | 0.8890 (4) | 0.8166 (3) | 0.2034 (4) | 0.0963 (15) | |
| Cl7 | 0.1337 (4) | 0.0699 (5) | 0.1131 (4) | 0.0819 (15) | 0.740 (3) |
| C61 | 0.1765 (12) | −0.0475 (9) | 0.2177 (8) | 0.0302 (3) | 0.740 (3) |
| H61A | 0.108903 | −0.089082 | 0.218036 | 0.036* | 0.740 (3) |
| H61B | 0.276777 | −0.101351 | 0.202280 | 0.036* | 0.740 (3) |
| Cl8 | 0.1656 (4) | −0.0086 (4) | 0.3389 (4) | 0.0645 (6) | 0.740 (3) |
| Cl7' | 0.129 (3) | −0.012 (3) | 0.087 (3) | 0.0963 (15) | 0.124 (3) |
| C61' | 0.249 (5) | 0.007 (7) | 0.168 (3) | 0.0302 (3) | 0.124 (3) |
| H61C | 0.332305 | −0.066406 | 0.178368 | 0.036* | 0.124 (3) |
| H61D | 0.287840 | 0.064322 | 0.128480 | 0.036* | 0.124 (3) |
| Cl8' | 0.178 (2) | 0.050 (2) | 0.2923 (19) | 0.0645 (6) | 0.124 (3) |
| Cl7" | 0.127 (2) | −0.0679 (19) | 0.166 (2) | 0.0645 (6) | 0.136 (3) |
| C61" | 0.276 (4) | −0.026 (3) | 0.178 (6) | 0.0302 (3) | 0.136 (3) |
| H61E | 0.327391 | −0.066354 | 0.242501 | 0.036* | 0.136 (3) |
| H61F | 0.345977 | −0.040293 | 0.115397 | 0.036* | 0.136 (3) |
| Cl8" | 0.191 (2) | 0.119 (2) | 0.187 (2) | 0.0819 (15) | 0.136 (3) |
trans-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane monosolvate (2) . Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Fe1 | 0.0152 (4) | 0.0115 (3) | 0.0147 (4) | −0.0053 (3) | −0.0038 (3) | −0.0015 (3) |
| Cl1 | 0.0180 (4) | 0.0166 (4) | 0.0190 (4) | −0.0078 (3) | −0.0047 (3) | −0.0020 (3) |
| Cl2 | 0.0180 (4) | 0.0166 (4) | 0.0190 (4) | −0.0078 (3) | −0.0047 (3) | −0.0020 (3) |
| P1 | 0.0166 (4) | 0.0123 (4) | 0.0160 (5) | −0.0052 (3) | −0.0034 (4) | −0.0018 (3) |
| P2 | 0.0181 (5) | 0.0128 (4) | 0.0151 (5) | −0.0064 (4) | −0.0035 (4) | −0.0012 (3) |
| P3 | 0.0166 (4) | 0.0123 (4) | 0.0160 (5) | −0.0052 (3) | −0.0034 (4) | −0.0018 (3) |
| P4 | 0.0181 (5) | 0.0128 (4) | 0.0151 (5) | −0.0064 (4) | −0.0035 (4) | −0.0012 (3) |
| C1 | 0.0207 (18) | 0.0144 (15) | 0.0161 (18) | −0.0071 (14) | −0.0032 (14) | −0.0003 (13) |
| C2 | 0.027 (2) | 0.0151 (16) | 0.021 (2) | −0.0076 (15) | −0.0045 (16) | −0.0037 (14) |
| C3 | 0.030 (2) | 0.0132 (16) | 0.024 (2) | −0.0072 (15) | −0.0075 (17) | −0.0012 (15) |
| C4 | 0.032 (2) | 0.0181 (17) | 0.022 (2) | −0.0130 (17) | −0.0054 (17) | 0.0039 (15) |
| C5 | 0.032 (2) | 0.0185 (18) | 0.020 (2) | −0.0115 (17) | −0.0020 (17) | −0.0025 (15) |
| C6 | 0.0188 (18) | 0.0146 (15) | 0.0169 (18) | −0.0053 (14) | −0.0030 (14) | −0.0020 (13) |
| C7 | 0.0207 (18) | 0.0116 (15) | 0.0191 (19) | −0.0052 (13) | −0.0045 (14) | −0.0017 (13) |
| C8 | 0.0198 (18) | 0.0149 (16) | 0.023 (2) | −0.0078 (14) | −0.0034 (15) | −0.0035 (14) |
| C9 | 0.031 (2) | 0.0160 (16) | 0.021 (2) | −0.0115 (16) | −0.0094 (16) | 0.0006 (14) |
| C10 | 0.040 (3) | 0.0204 (19) | 0.019 (2) | −0.0132 (18) | −0.0048 (18) | −0.0042 (15) |
| C11 | 0.033 (2) | 0.029 (2) | 0.023 (2) | −0.0135 (19) | 0.0038 (18) | −0.0086 (18) |
| C12 | 0.022 (2) | 0.0203 (19) | 0.023 (2) | −0.0073 (16) | −0.0021 (16) | −0.0038 (15) |
| C13 | 0.0206 (19) | 0.0171 (17) | 0.024 (2) | −0.0051 (15) | −0.0047 (15) | −0.0046 (14) |
| C14 | 0.022 (2) | 0.0182 (18) | 0.033 (2) | −0.0090 (15) | −0.0062 (17) | −0.0031 (16) |
| C15 | 0.020 (2) | 0.029 (2) | 0.042 (3) | −0.0091 (18) | −0.0049 (19) | −0.012 (2) |
| C16 | 0.019 (2) | 0.029 (2) | 0.042 (3) | −0.0007 (17) | −0.0151 (19) | −0.008 (2) |
| C17 | 0.030 (3) | 0.029 (2) | 0.040 (3) | 0.0013 (19) | −0.019 (2) | 0.003 (2) |
| C18 | 0.026 (2) | 0.023 (2) | 0.028 (2) | −0.0032 (17) | −0.0068 (18) | 0.0002 (17) |
| C19 | 0.0190 (19) | 0.0193 (17) | 0.0110 (17) | −0.0068 (15) | −0.0015 (14) | −0.0008 (13) |
| C20 | 0.029 (2) | 0.020 (2) | 0.025 (2) | −0.0047 (17) | −0.0074 (17) | −0.0054 (17) |
| C21 | 0.027 (2) | 0.026 (2) | 0.031 (3) | −0.0029 (19) | −0.0128 (19) | −0.0014 (19) |
| C22 | 0.029 (2) | 0.035 (2) | 0.017 (2) | −0.014 (2) | −0.0094 (18) | 0.0011 (17) |
| C23 | 0.024 (2) | 0.026 (2) | 0.017 (2) | −0.0141 (19) | 0.0009 (17) | −0.0056 (16) |
| C24 | 0.019 (2) | 0.0191 (17) | 0.020 (2) | −0.0105 (16) | −0.0017 (16) | 0.0001 (14) |
| C25 | 0.0182 (18) | 0.0185 (17) | 0.0173 (19) | −0.0081 (14) | −0.0023 (14) | −0.0002 (13) |
| C26 | 0.022 (2) | 0.027 (2) | 0.027 (2) | −0.0099 (17) | −0.0006 (17) | −0.0070 (17) |
| C27 | 0.026 (2) | 0.040 (3) | 0.038 (3) | −0.012 (2) | 0.006 (2) | −0.013 (2) |
| C28 | 0.023 (2) | 0.043 (3) | 0.041 (3) | −0.017 (2) | 0.005 (2) | −0.007 (2) |
| C29 | 0.024 (2) | 0.034 (2) | 0.038 (3) | −0.019 (2) | −0.007 (2) | 0.002 (2) |
| C30 | 0.028 (2) | 0.026 (2) | 0.021 (2) | −0.0169 (17) | −0.0042 (16) | 0.0003 (16) |
| C31 | 0.0207 (18) | 0.0144 (15) | 0.0161 (18) | −0.0071 (14) | −0.0032 (14) | −0.0003 (13) |
| C32 | 0.027 (2) | 0.0151 (16) | 0.021 (2) | −0.0076 (15) | −0.0045 (16) | −0.0037 (14) |
| C33 | 0.030 (2) | 0.0132 (16) | 0.024 (2) | −0.0072 (15) | −0.0075 (17) | −0.0012 (15) |
| C34 | 0.032 (2) | 0.0181 (17) | 0.022 (2) | −0.0130 (17) | −0.0054 (17) | 0.0039 (15) |
| C35 | 0.032 (2) | 0.0185 (18) | 0.020 (2) | −0.0115 (17) | −0.0020 (17) | −0.0025 (15) |
| C36 | 0.0188 (18) | 0.0146 (15) | 0.0169 (18) | −0.0053 (14) | −0.0030 (14) | −0.0020 (13) |
| C37 | 0.0207 (18) | 0.0116 (15) | 0.0191 (19) | −0.0052 (13) | −0.0045 (14) | −0.0017 (13) |
| C38 | 0.0198 (18) | 0.0149 (16) | 0.023 (2) | −0.0078 (14) | −0.0034 (15) | −0.0035 (14) |
| C39 | 0.031 (2) | 0.0160 (16) | 0.021 (2) | −0.0115 (16) | −0.0094 (16) | 0.0006 (14) |
| C40 | 0.040 (3) | 0.0204 (19) | 0.019 (2) | −0.0132 (18) | −0.0048 (18) | −0.0042 (15) |
| C41 | 0.033 (2) | 0.029 (2) | 0.023 (2) | −0.0135 (19) | 0.0038 (18) | −0.0086 (18) |
| C42 | 0.022 (2) | 0.0203 (19) | 0.023 (2) | −0.0073 (16) | −0.0021 (16) | −0.0038 (15) |
| C43 | 0.0206 (19) | 0.0171 (17) | 0.024 (2) | −0.0051 (15) | −0.0047 (15) | −0.0046 (14) |
| C44 | 0.022 (2) | 0.0182 (18) | 0.033 (2) | −0.0090 (15) | −0.0062 (17) | −0.0031 (16) |
| C45 | 0.020 (2) | 0.029 (2) | 0.042 (3) | −0.0091 (18) | −0.0049 (19) | −0.012 (2) |
| C46 | 0.019 (2) | 0.029 (2) | 0.042 (3) | −0.0007 (17) | −0.0151 (19) | −0.008 (2) |
| C47 | 0.030 (3) | 0.029 (2) | 0.040 (3) | 0.0013 (19) | −0.019 (2) | 0.003 (2) |
| C48 | 0.026 (2) | 0.023 (2) | 0.028 (2) | −0.0032 (17) | −0.0068 (18) | 0.0002 (17) |
| C49 | 0.0190 (19) | 0.0193 (17) | 0.0110 (17) | −0.0068 (15) | −0.0015 (14) | −0.0008 (13) |
| C50 | 0.029 (2) | 0.020 (2) | 0.025 (2) | −0.0047 (17) | −0.0074 (17) | −0.0054 (17) |
| C51 | 0.027 (2) | 0.026 (2) | 0.031 (3) | −0.0029 (19) | −0.0128 (19) | −0.0014 (19) |
| C52 | 0.029 (2) | 0.035 (2) | 0.017 (2) | −0.014 (2) | −0.0094 (18) | 0.0011 (17) |
| C53 | 0.024 (2) | 0.026 (2) | 0.017 (2) | −0.0141 (19) | 0.0009 (17) | −0.0056 (16) |
| C54 | 0.019 (2) | 0.0191 (17) | 0.020 (2) | −0.0105 (16) | −0.0017 (16) | 0.0001 (14) |
| C55 | 0.0182 (18) | 0.0185 (17) | 0.0173 (19) | −0.0081 (14) | −0.0023 (14) | −0.0002 (13) |
| C56 | 0.022 (2) | 0.027 (2) | 0.027 (2) | −0.0099 (17) | −0.0006 (17) | −0.0070 (17) |
| C57 | 0.026 (2) | 0.040 (3) | 0.038 (3) | −0.012 (2) | 0.006 (2) | −0.013 (2) |
| C58 | 0.023 (2) | 0.043 (3) | 0.041 (3) | −0.017 (2) | 0.005 (2) | −0.007 (2) |
| C59 | 0.024 (2) | 0.034 (2) | 0.038 (3) | −0.019 (2) | −0.007 (2) | 0.002 (2) |
| C60 | 0.028 (2) | 0.026 (2) | 0.021 (2) | −0.0169 (17) | −0.0042 (16) | 0.0003 (16) |
| Fe2 | 0.0234 (6) | 0.0251 (6) | 0.0393 (7) | −0.0018 (4) | −0.0095 (5) | −0.0077 (5) |
| Cl3 | 0.0226 (9) | 0.0378 (11) | 0.0356 (12) | −0.0001 (8) | −0.0087 (8) | −0.0093 (9) |
| Cl4 | 0.0709 (17) | 0.0271 (10) | 0.0283 (11) | −0.0138 (11) | 0.0042 (11) | −0.0046 (8) |
| Cl5 | 0.0335 (9) | 0.0725 (13) | 0.0668 (13) | −0.0075 (9) | 0.0006 (8) | 0.0200 (10) |
| Cl6 | 0.0488 (16) | 0.090 (2) | 0.146 (3) | 0.0219 (15) | −0.0621 (19) | −0.077 (2) |
| Cl7 | 0.0330 (19) | 0.128 (4) | 0.070 (3) | −0.006 (2) | −0.0002 (18) | −0.027 (3) |
| C61 | 0.0234 (6) | 0.0251 (6) | 0.0393 (7) | −0.0018 (4) | −0.0095 (5) | −0.0077 (5) |
| Cl8 | 0.0335 (9) | 0.0725 (13) | 0.0668 (13) | −0.0075 (9) | 0.0006 (8) | 0.0200 (10) |
| Cl7' | 0.0488 (16) | 0.090 (2) | 0.146 (3) | 0.0219 (15) | −0.0621 (19) | −0.077 (2) |
| C61' | 0.0234 (6) | 0.0251 (6) | 0.0393 (7) | −0.0018 (4) | −0.0095 (5) | −0.0077 (5) |
| Cl8' | 0.0335 (9) | 0.0725 (13) | 0.0668 (13) | −0.0075 (9) | 0.0006 (8) | 0.0200 (10) |
| Cl7" | 0.0335 (9) | 0.0725 (13) | 0.0668 (13) | −0.0075 (9) | 0.0006 (8) | 0.0200 (10) |
| C61" | 0.0234 (6) | 0.0251 (6) | 0.0393 (7) | −0.0018 (4) | −0.0095 (5) | −0.0077 (5) |
| Cl8" | 0.0330 (19) | 0.128 (4) | 0.070 (3) | −0.006 (2) | −0.0002 (18) | −0.027 (3) |
trans-Bis[1,2-bis(diphenylphosphane)benzene]dichloridoiron(III) tetrachloridoferrate(III) dichloromethane monosolvate (2) . Geometric parameters (Å, º)
| Fe1—Cl2 | 2.218 (2) | C30—H30 | 0.9500 |
| Fe1—Cl1 | 2.223 (2) | C31—C36 | 1.376 (11) |
| Fe1—P3 | 2.374 (2) | C31—C32 | 1.410 (10) |
| Fe1—P2 | 2.376 (2) | C32—C33 | 1.377 (11) |
| Fe1—P4 | 2.377 (2) | C32—H32 | 0.9500 |
| Fe1—P1 | 2.388 (2) | C33—C34 | 1.396 (12) |
| P1—C1 | 1.810 (8) | C33—H33 | 0.9500 |
| P1—C7 | 1.827 (8) | C34—C35 | 1.374 (11) |
| P1—C13 | 1.830 (8) | C34—H34 | 0.9500 |
| P2—C25 | 1.817 (8) | C35—C36 | 1.408 (11) |
| P2—C19 | 1.819 (8) | C35—H35 | 0.9500 |
| P2—C6 | 1.822 (7) | C37—C38 | 1.393 (11) |
| P3—C37 | 1.828 (8) | C37—C42 | 1.404 (11) |
| P3—C43 | 1.830 (8) | C38—C39 | 1.379 (11) |
| P3—C31 | 1.833 (8) | C38—H38 | 0.9500 |
| P4—C36 | 1.811 (7) | C39—C40 | 1.398 (13) |
| P4—C49 | 1.834 (8) | C39—H39 | 0.9500 |
| P4—C55 | 1.835 (8) | C40—C41 | 1.387 (12) |
| C1—C2 | 1.403 (10) | C40—H40 | 0.9500 |
| C1—C6 | 1.410 (11) | C41—C42 | 1.389 (11) |
| C2—C3 | 1.404 (11) | C41—H41 | 0.9500 |
| C2—H2 | 0.9500 | C42—H42 | 0.9500 |
| C3—C4 | 1.373 (12) | C43—C44 | 1.406 (11) |
| C3—H3 | 0.9500 | C43—C48 | 1.411 (12) |
| C4—C5 | 1.399 (11) | C44—C45 | 1.362 (11) |
| C4—H4 | 0.9500 | C44—H44 | 0.9500 |
| C5—C6 | 1.396 (11) | C45—C46 | 1.415 (13) |
| C5—H5 | 0.9500 | C45—H45 | 0.9500 |
| C7—C12 | 1.387 (11) | C46—C47 | 1.355 (13) |
| C7—C8 | 1.421 (11) | C46—H46 | 0.9500 |
| C8—C9 | 1.379 (10) | C47—C48 | 1.371 (12) |
| C8—H8 | 0.9500 | C47—H47 | 0.9500 |
| C9—C10 | 1.367 (12) | C48—H48 | 0.9500 |
| C9—H9 | 0.9500 | C49—C50 | 1.382 (11) |
| C10—C11 | 1.379 (12) | C49—C54 | 1.404 (10) |
| C10—H10 | 0.9500 | C50—C51 | 1.398 (12) |
| C11—C12 | 1.406 (11) | C50—H50 | 0.9500 |
| C11—H11 | 0.9500 | C51—C52 | 1.398 (11) |
| C12—H12 | 0.9500 | C51—H51 | 0.9500 |
| C13—C14 | 1.374 (11) | C52—C53 | 1.377 (12) |
| C13—C18 | 1.392 (12) | C52—H52 | 0.9500 |
| C14—C15 | 1.394 (11) | C53—C54 | 1.395 (11) |
| C14—H14 | 0.9500 | C53—H53 | 0.9500 |
| C15—C16 | 1.352 (13) | C54—H54 | 0.9500 |
| C15—H15 | 0.9500 | C55—C56 | 1.388 (11) |
| C16—C17 | 1.411 (14) | C55—C60 | 1.396 (11) |
| C16—H16 | 0.9500 | C56—C57 | 1.378 (12) |
| C17—C18 | 1.400 (12) | C56—H56 | 0.9500 |
| C17—H17 | 0.9500 | C57—C58 | 1.367 (12) |
| C18—H18 | 0.9500 | C57—H57 | 0.9500 |
| C19—C24 | 1.392 (10) | C58—C59 | 1.394 (13) |
| C19—C20 | 1.394 (11) | C58—H58 | 0.9500 |
| C20—C21 | 1.365 (12) | C59—C60 | 1.385 (12) |
| C20—H20 | 0.9500 | C59—H59 | 0.9500 |
| C21—C22 | 1.392 (12) | C60—H60 | 0.9500 |
| C21—H21 | 0.9500 | Fe2—Cl4 | 2.184 (2) |
| C22—C23 | 1.384 (12) | Fe2—Cl5 | 2.188 (3) |
| C22—H22 | 0.9500 | Fe2—Cl3 | 2.193 (2) |
| C23—C24 | 1.385 (11) | Fe2—Cl6 | 2.197 (3) |
| C23—H23 | 0.9500 | Cl7—C61 | 1.799 (11) |
| C24—H24 | 0.9500 | C61—Cl8 | 1.682 (10) |
| C25—C26 | 1.399 (11) | C61—H61A | 0.9900 |
| C25—C30 | 1.406 (11) | C61—H61B | 0.9900 |
| C26—C27 | 1.397 (12) | Cl7'—C61' | 1.77 (2) |
| C26—H26 | 0.9500 | C61'—Cl8' | 1.75 (2) |
| C27—C28 | 1.420 (13) | C61'—H61C | 0.9900 |
| C27—H27 | 0.9500 | C61'—H61D | 0.9900 |
| C28—C29 | 1.354 (13) | Cl7"—C61" | 1.76 (2) |
| C28—H28 | 0.9500 | C61"—Cl8" | 1.73 (2) |
| C29—C30 | 1.394 (12) | C61"—H61E | 0.9900 |
| C29—H29 | 0.9500 | C61"—H61F | 0.9900 |
| Cl2—Fe1—Cl1 | 179.87 (12) | C27—C28—H28 | 119.4 |
| Cl2—Fe1—P3 | 87.69 (8) | C28—C29—C30 | 120.1 (8) |
| Cl1—Fe1—P3 | 92.26 (8) | C28—C29—H29 | 119.9 |
| Cl2—Fe1—P2 | 92.82 (8) | C30—C29—H29 | 119.9 |
| Cl1—Fe1—P2 | 87.30 (8) | C29—C30—C25 | 120.7 (8) |
| P3—Fe1—P2 | 98.58 (8) | C29—C30—H30 | 119.7 |
| Cl2—Fe1—P4 | 87.23 (8) | C25—C30—H30 | 119.7 |
| Cl1—Fe1—P4 | 92.65 (8) | C36—C31—C32 | 121.2 (7) |
| P3—Fe1—P4 | 80.75 (8) | C36—C31—P3 | 117.5 (6) |
| P2—Fe1—P4 | 179.33 (10) | C32—C31—P3 | 121.2 (6) |
| Cl2—Fe1—P1 | 92.05 (8) | C33—C32—C31 | 119.3 (7) |
| Cl1—Fe1—P1 | 87.99 (7) | C33—C32—H32 | 120.4 |
| P3—Fe1—P1 | 179.74 (10) | C31—C32—H32 | 120.4 |
| P2—Fe1—P1 | 81.38 (8) | C32—C33—C34 | 119.9 (7) |
| P4—Fe1—P1 | 99.29 (8) | C32—C33—H33 | 120.1 |
| C1—P1—C7 | 100.8 (3) | C34—C33—H33 | 120.1 |
| C1—P1—C13 | 103.2 (4) | C35—C34—C33 | 120.7 (8) |
| C7—P1—C13 | 105.0 (4) | C35—C34—H34 | 119.7 |
| C1—P1—Fe1 | 107.7 (3) | C33—C34—H34 | 119.7 |
| C7—P1—Fe1 | 120.0 (3) | C34—C35—C36 | 120.3 (8) |
| C13—P1—Fe1 | 117.6 (2) | C34—C35—H35 | 119.9 |
| C25—P2—C19 | 105.8 (4) | C36—C35—H35 | 119.9 |
| C25—P2—C6 | 100.4 (4) | C31—C36—C35 | 118.7 (7) |
| C19—P2—C6 | 102.7 (4) | C31—C36—P4 | 118.2 (6) |
| C25—P2—Fe1 | 120.0 (3) | C35—C36—P4 | 122.9 (6) |
| C19—P2—Fe1 | 117.0 (3) | C38—C37—C42 | 118.3 (7) |
| C6—P2—Fe1 | 108.3 (3) | C38—C37—P3 | 119.4 (6) |
| C37—P3—C43 | 104.8 (4) | C42—C37—P3 | 122.3 (6) |
| C37—P3—C31 | 100.6 (3) | C39—C38—C37 | 121.6 (8) |
| C43—P3—C31 | 103.8 (4) | C39—C38—H38 | 119.2 |
| C37—P3—Fe1 | 119.4 (3) | C37—C38—H38 | 119.2 |
| C43—P3—Fe1 | 118.2 (2) | C38—C39—C40 | 119.7 (8) |
| C31—P3—Fe1 | 107.7 (3) | C38—C39—H39 | 120.2 |
| C36—P4—C49 | 102.8 (4) | C40—C39—H39 | 120.2 |
| C36—P4—C55 | 101.4 (4) | C41—C40—C39 | 119.7 (8) |
| C49—P4—C55 | 107.0 (4) | C41—C40—H40 | 120.1 |
| C36—P4—Fe1 | 108.0 (3) | C39—C40—H40 | 120.1 |
| C49—P4—Fe1 | 116.1 (3) | C40—C41—C42 | 120.3 (8) |
| C55—P4—Fe1 | 119.2 (3) | C40—C41—H41 | 119.9 |
| C2—C1—C6 | 119.1 (7) | C42—C41—H41 | 119.9 |
| C2—C1—P1 | 122.3 (6) | C41—C42—C37 | 120.5 (8) |
| C6—C1—P1 | 118.5 (6) | C41—C42—H42 | 119.8 |
| C1—C2—C3 | 119.3 (7) | C37—C42—H42 | 119.8 |
| C1—C2—H2 | 120.3 | C44—C43—C48 | 117.6 (8) |
| C3—C2—H2 | 120.3 | C44—C43—P3 | 119.8 (6) |
| C4—C3—C2 | 121.2 (7) | C48—C43—P3 | 122.6 (7) |
| C4—C3—H3 | 119.4 | C45—C44—C43 | 122.0 (9) |
| C2—C3—H3 | 119.4 | C45—C44—H44 | 119.0 |
| C3—C4—C5 | 120.3 (8) | C43—C44—H44 | 119.0 |
| C3—C4—H4 | 119.8 | C44—C45—C46 | 118.7 (9) |
| C5—C4—H4 | 119.8 | C44—C45—H45 | 120.6 |
| C6—C5—C4 | 119.3 (8) | C46—C45—H45 | 120.6 |
| C6—C5—H5 | 120.3 | C47—C46—C45 | 119.9 (8) |
| C4—C5—H5 | 120.3 | C47—C46—H46 | 120.0 |
| C5—C6—C1 | 120.7 (7) | C45—C46—H46 | 120.0 |
| C5—C6—P2 | 122.0 (6) | C46—C47—C48 | 121.8 (9) |
| C1—C6—P2 | 117.2 (6) | C46—C47—H47 | 119.1 |
| C12—C7—C8 | 118.7 (7) | C48—C47—H47 | 119.1 |
| C12—C7—P1 | 123.3 (6) | C47—C48—C43 | 119.9 (9) |
| C8—C7—P1 | 118.1 (6) | C47—C48—H48 | 120.1 |
| C9—C8—C7 | 119.9 (8) | C43—C48—H48 | 120.1 |
| C9—C8—H8 | 120.0 | C50—C49—C54 | 119.9 (7) |
| C7—C8—H8 | 120.0 | C50—C49—P4 | 121.2 (6) |
| C10—C9—C8 | 121.1 (8) | C54—C49—P4 | 118.9 (6) |
| C10—C9—H9 | 119.5 | C49—C50—C51 | 120.0 (7) |
| C8—C9—H9 | 119.5 | C49—C50—H50 | 120.0 |
| C9—C10—C11 | 120.0 (8) | C51—C50—H50 | 120.0 |
| C9—C10—H10 | 120.0 | C50—C51—C52 | 120.0 (8) |
| C11—C10—H10 | 120.0 | C50—C51—H51 | 120.0 |
| C10—C11—C12 | 120.4 (8) | C52—C51—H51 | 120.0 |
| C10—C11—H11 | 119.8 | C53—C52—C51 | 119.8 (8) |
| C12—C11—H11 | 119.8 | C53—C52—H52 | 120.1 |
| C7—C12—C11 | 119.9 (8) | C51—C52—H52 | 120.1 |
| C7—C12—H12 | 120.1 | C52—C53—C54 | 120.6 (7) |
| C11—C12—H12 | 120.1 | C52—C53—H53 | 119.7 |
| C14—C13—C18 | 119.0 (8) | C54—C53—H53 | 119.7 |
| C14—C13—P1 | 119.4 (7) | C53—C54—C49 | 119.6 (8) |
| C18—C13—P1 | 121.6 (7) | C53—C54—H54 | 120.2 |
| C13—C14—C15 | 120.8 (9) | C49—C54—H54 | 120.2 |
| C13—C14—H14 | 119.6 | C56—C55—C60 | 118.6 (8) |
| C15—C14—H14 | 119.6 | C56—C55—P4 | 122.9 (6) |
| C16—C15—C14 | 120.8 (9) | C60—C55—P4 | 118.4 (6) |
| C16—C15—H15 | 119.6 | C57—C56—C55 | 120.7 (8) |
| C14—C15—H15 | 119.6 | C57—C56—H56 | 119.6 |
| C15—C16—C17 | 119.9 (8) | C55—C56—H56 | 119.6 |
| C15—C16—H16 | 120.0 | C58—C57—C56 | 121.1 (9) |
| C17—C16—H16 | 120.0 | C58—C57—H57 | 119.5 |
| C18—C17—C16 | 119.0 (9) | C56—C57—H57 | 119.5 |
| C18—C17—H17 | 120.5 | C57—C58—C59 | 118.9 (9) |
| C16—C17—H17 | 120.5 | C57—C58—H58 | 120.5 |
| C13—C18—C17 | 120.5 (9) | C59—C58—H58 | 120.5 |
| C13—C18—H18 | 119.8 | C60—C59—C58 | 120.6 (8) |
| C17—C18—H18 | 119.8 | C60—C59—H59 | 119.7 |
| C24—C19—C20 | 117.5 (7) | C58—C59—H59 | 119.7 |
| C24—C19—P2 | 121.4 (6) | C59—C60—C55 | 120.0 (8) |
| C20—C19—P2 | 121.0 (6) | C59—C60—H60 | 120.0 |
| C21—C20—C19 | 121.1 (8) | C55—C60—H60 | 120.0 |
| C21—C20—H20 | 119.4 | Cl4—Fe2—Cl5 | 109.67 (12) |
| C19—C20—H20 | 119.4 | Cl4—Fe2—Cl3 | 108.95 (10) |
| C20—C21—C22 | 121.0 (8) | Cl5—Fe2—Cl3 | 110.14 (11) |
| C20—C21—H21 | 119.5 | Cl4—Fe2—Cl6 | 110.12 (15) |
| C22—C21—H21 | 119.5 | Cl5—Fe2—Cl6 | 110.26 (17) |
| C23—C22—C21 | 118.8 (8) | Cl3—Fe2—Cl6 | 107.67 (10) |
| C23—C22—H22 | 120.6 | Cl8—C61—Cl7 | 114.4 (6) |
| C21—C22—H22 | 120.6 | Cl8—C61—H61A | 108.7 |
| C22—C23—C24 | 119.8 (7) | Cl7—C61—H61A | 108.7 |
| C22—C23—H23 | 120.1 | Cl8—C61—H61B | 108.7 |
| C24—C23—H23 | 120.1 | Cl7—C61—H61B | 108.7 |
| C23—C24—C19 | 121.7 (8) | H61A—C61—H61B | 107.6 |
| C23—C24—H24 | 119.2 | Cl8'—C61'—Cl7' | 117 (3) |
| C19—C24—H24 | 119.2 | Cl8'—C61'—H61C | 107.9 |
| C26—C25—C30 | 118.6 (8) | Cl7'—C61'—H61C | 107.9 |
| C26—C25—P2 | 123.1 (6) | Cl8'—C61'—H61D | 107.9 |
| C30—C25—P2 | 118.2 (6) | Cl7'—C61'—H61D | 107.9 |
| C27—C26—C25 | 120.8 (8) | H61C—C61'—H61D | 107.2 |
| C27—C26—H26 | 119.6 | Cl8"—C61"—Cl7" | 102 (2) |
| C25—C26—H26 | 119.6 | Cl8"—C61"—H61E | 111.3 |
| C26—C27—C28 | 118.4 (8) | Cl7"—C61"—H61E | 111.3 |
| C26—C27—H27 | 120.8 | Cl8"—C61"—H61F | 111.3 |
| C28—C27—H27 | 120.8 | Cl7"—C61"—H61F | 111.3 |
| C29—C28—C27 | 121.2 (9) | H61E—C61"—H61F | 109.2 |
| C29—C28—H28 | 119.4 | ||
| C7—P1—C1—C2 | −37.2 (7) | C37—P3—C31—C36 | −145.7 (6) |
| C13—P1—C1—C2 | 71.2 (7) | C43—P3—C31—C36 | 106.0 (7) |
| Fe1—P1—C1—C2 | −163.7 (6) | Fe1—P3—C31—C36 | −20.1 (7) |
| C7—P1—C1—C6 | 145.8 (6) | C37—P3—C31—C32 | 38.2 (7) |
| C13—P1—C1—C6 | −105.7 (7) | C43—P3—C31—C32 | −70.1 (7) |
| Fe1—P1—C1—C6 | 19.3 (7) | Fe1—P3—C31—C32 | 163.8 (6) |
| C6—C1—C2—C3 | 1.5 (12) | C36—C31—C32—C33 | 0.1 (12) |
| P1—C1—C2—C3 | −175.5 (6) | P3—C31—C32—C33 | 176.0 (6) |
| C1—C2—C3—C4 | −1.5 (13) | C31—C32—C33—C34 | 0.0 (13) |
| C2—C3—C4—C5 | 0.9 (13) | C32—C33—C34—C35 | −0.6 (13) |
| C3—C4—C5—C6 | −0.2 (13) | C33—C34—C35—C36 | 1.2 (13) |
| C4—C5—C6—C1 | 0.2 (12) | C32—C31—C36—C35 | 0.5 (12) |
| C4—C5—C6—P2 | 177.1 (7) | P3—C31—C36—C35 | −175.6 (6) |
| C2—C1—C6—C5 | −0.9 (12) | C32—C31—C36—P4 | 176.2 (6) |
| P1—C1—C6—C5 | 176.2 (6) | P3—C31—C36—P4 | 0.1 (9) |
| C2—C1—C6—P2 | −177.9 (6) | C34—C35—C36—C31 | −1.2 (12) |
| P1—C1—C6—P2 | −0.9 (9) | C34—C35—C36—P4 | −176.6 (7) |
| C25—P2—C6—C5 | 38.1 (8) | C49—P4—C36—C31 | −103.3 (7) |
| C19—P2—C6—C5 | −70.8 (7) | C55—P4—C36—C31 | 146.1 (7) |
| Fe1—P2—C6—C5 | 164.8 (6) | Fe1—P4—C36—C31 | 20.0 (7) |
| C25—P2—C6—C1 | −144.8 (6) | C49—P4—C36—C35 | 72.2 (7) |
| C19—P2—C6—C1 | 106.2 (7) | C55—P4—C36—C35 | −38.4 (8) |
| Fe1—P2—C6—C1 | −18.2 (7) | Fe1—P4—C36—C35 | −164.6 (6) |
| C1—P1—C7—C12 | 128.4 (7) | C43—P3—C37—C38 | 155.9 (6) |
| C13—P1—C7—C12 | 21.4 (8) | C31—P3—C37—C38 | 48.5 (7) |
| Fe1—P1—C7—C12 | −113.8 (6) | Fe1—P3—C37—C38 | −68.9 (7) |
| C1—P1—C7—C8 | −51.5 (7) | C43—P3—C37—C42 | −23.3 (8) |
| C13—P1—C7—C8 | −158.6 (6) | C31—P3—C37—C42 | −130.7 (7) |
| Fe1—P1—C7—C8 | 66.3 (7) | Fe1—P3—C37—C42 | 111.9 (6) |
| C12—C7—C8—C9 | 2.1 (11) | C42—C37—C38—C39 | −2.0 (11) |
| P1—C7—C8—C9 | −177.9 (6) | P3—C37—C38—C39 | 178.8 (6) |
| C7—C8—C9—C10 | −1.2 (12) | C37—C38—C39—C40 | 0.1 (12) |
| C8—C9—C10—C11 | −0.1 (13) | C38—C39—C40—C41 | 1.4 (13) |
| C9—C10—C11—C12 | 0.6 (13) | C39—C40—C41—C42 | −1.0 (13) |
| C8—C7—C12—C11 | −1.6 (12) | C40—C41—C42—C37 | −1.0 (13) |
| P1—C7—C12—C11 | 178.4 (6) | C38—C37—C42—C41 | 2.4 (12) |
| C10—C11—C12—C7 | 0.3 (13) | P3—C37—C42—C41 | −178.3 (6) |
| C1—P1—C13—C14 | −179.5 (6) | C37—P3—C43—C44 | 77.3 (7) |
| C7—P1—C13—C14 | −74.3 (7) | C31—P3—C43—C44 | −177.6 (6) |
| Fe1—P1—C13—C14 | 62.2 (7) | Fe1—P3—C43—C44 | −58.5 (7) |
| C1—P1—C13—C18 | 0.4 (8) | C37—P3—C43—C48 | −105.1 (7) |
| C7—P1—C13—C18 | 105.7 (7) | C31—P3—C43—C48 | −0.1 (8) |
| Fe1—P1—C13—C18 | −117.9 (6) | Fe1—P3—C43—C48 | 119.0 (6) |
| C18—C13—C14—C15 | 0.0 (12) | C48—C43—C44—C45 | 2.1 (12) |
| P1—C13—C14—C15 | 180.0 (6) | P3—C43—C44—C45 | 179.7 (6) |
| C13—C14—C15—C16 | 1.0 (13) | C43—C44—C45—C46 | −1.7 (13) |
| C14—C15—C16—C17 | −0.8 (13) | C44—C45—C46—C47 | 1.3 (13) |
| C15—C16—C17—C18 | −0.4 (13) | C45—C46—C47—C48 | −1.4 (14) |
| C14—C13—C18—C17 | −1.2 (13) | C46—C47—C48—C43 | 1.8 (14) |
| P1—C13—C18—C17 | 178.8 (7) | C44—C43—C48—C47 | −2.1 (12) |
| C16—C17—C18—C13 | 1.4 (13) | P3—C43—C48—C47 | −179.7 (7) |
| C25—P2—C19—C24 | 66.4 (7) | C36—P4—C49—C50 | 7.1 (8) |
| C6—P2—C19—C24 | 171.3 (6) | C55—P4—C49—C50 | 113.5 (7) |
| Fe1—P2—C19—C24 | −70.3 (7) | Fe1—P4—C49—C50 | −110.5 (7) |
| C25—P2—C19—C20 | −118.1 (7) | C36—P4—C49—C54 | −174.0 (6) |
| C6—P2—C19—C20 | −13.3 (8) | C55—P4—C49—C54 | −67.6 (7) |
| Fe1—P2—C19—C20 | 105.2 (7) | Fe1—P4—C49—C54 | 68.4 (7) |
| C24—C19—C20—C21 | −1.5 (13) | C54—C49—C50—C51 | −0.6 (13) |
| P2—C19—C20—C21 | −177.1 (7) | P4—C49—C50—C51 | 178.3 (7) |
| C19—C20—C21—C22 | −1.7 (14) | C49—C50—C51—C52 | 0.7 (14) |
| C20—C21—C22—C23 | 2.4 (14) | C50—C51—C52—C53 | 0.7 (14) |
| C21—C22—C23—C24 | 0.0 (12) | C51—C52—C53—C54 | −2.3 (13) |
| C22—C23—C24—C19 | −3.3 (12) | C52—C53—C54—C49 | 2.5 (12) |
| C20—C19—C24—C23 | 4.0 (12) | C50—C49—C54—C53 | −1.0 (12) |
| P2—C19—C24—C23 | 179.6 (6) | P4—C49—C54—C53 | −179.9 (6) |
| C19—P2—C25—C26 | −29.2 (8) | C36—P4—C55—C56 | 139.5 (7) |
| C6—P2—C25—C26 | −135.8 (7) | C49—P4—C55—C56 | 32.2 (8) |
| Fe1—P2—C25—C26 | 105.9 (7) | Fe1—P4—C55—C56 | −102.1 (7) |
| C19—P2—C25—C30 | 151.7 (7) | C36—P4—C55—C60 | −42.9 (7) |
| C6—P2—C25—C30 | 45.2 (7) | C49—P4—C55—C60 | −150.2 (7) |
| Fe1—P2—C25—C30 | −73.2 (7) | Fe1—P4—C55—C60 | 75.4 (7) |
| C30—C25—C26—C27 | 3.6 (13) | C60—C55—C56—C57 | −1.2 (13) |
| P2—C25—C26—C27 | −175.4 (7) | P4—C55—C56—C57 | 176.3 (7) |
| C25—C26—C27—C28 | −1.8 (14) | C55—C56—C57—C58 | 0.0 (15) |
| C26—C27—C28—C29 | −1.5 (15) | C56—C57—C58—C59 | 1.7 (16) |
| C27—C28—C29—C30 | 3.0 (16) | C57—C58—C59—C60 | −2.2 (15) |
| C28—C29—C30—C25 | −1.1 (14) | C58—C59—C60—C55 | 1.0 (14) |
| C26—C25—C30—C29 | −2.2 (13) | C56—C55—C60—C59 | 0.7 (13) |
| P2—C25—C30—C29 | 176.9 (7) | P4—C55—C60—C59 | −177.0 (7) |
Funding Statement
This work was funded by National Science Foundation, Division of Chemistry grant CHE-1454370 to Michael L. Neidig.
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablock(s) 1, 2, global. DOI: 10.1107/S2056989018006898/pj2052sup1.cif
Structure factors: contains datablock(s) 1. DOI: 10.1107/S2056989018006898/pj20521sup2.hkl
Structure factors: contains datablock(s) 2. DOI: 10.1107/S2056989018006898/pj20522sup3.hkl
Additional supporting information: crystallographic information; 3D view; checkCIF report