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Acta Cryst. (2002). C58, m116-m118
https://doi.org/10.1107/S0108270101019370
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[μ-1κ2O,O′:2(η5)-Cyclopentadienylcarboxylato][2(η5)-diphenylphosphinocyclopentadienyl]bis[1,1(η5)-tetramethylcyclopentadienyl]iron(II)titanium(III)

K. Mach, J. Kubišta, I. Císařová and P. Štěpnička
Reacting stoichiometric amounts of 1-(diphenylphosphino)ferrocene­carboxylic acid and [Ti(η5-C5HMe4)2(η2-Me3SiC[triple bond]CSiMe3)] produced the title carboxyl­atotitanocene complex, [{μ-1κ2O,O′:2(η5)-C5H4CO2}{2(η5)-C5H4P(C6H5)2}{1(η5)-C5H(CH3)4}2FeIITiIII] or [FeTi(C9H13)2(C6H4O2)(C17H14P)]. The angle subtended by the Ti/O/O′ plane, where O and O′ are the donor atoms of the κ2-carboxy­late group, and the plane of the carboxyl-substituted ferrocene cyclo­penta­dienyl is 24.93 (6)°.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101019370/gd1183sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101019370/gd1183Isup2.hkl
Contains datablock I

CCDC reference: 181999

Comment top

Multidentate ligands possessing donor groups of different nature according to Pearson's HSAB concept (so-called hybrid ligands) Please define HSAB and provide a reference are capable of hemilabile coordination and of linking (different) transition metals into multinuclear complexes. Whereas the former property plays an important role in homogeneous catalysis, the latter is relevant mainly to fundamental research and material chemistry.

We have recently reported the synthesis of a ferrocene carboxyphosphine ligand, 1'-(diphenylphosphino)ferrocenecarboxylic acid (Hdpf; Podlaha et al., 1995), and its coordination properties towards various metals (Štěpnička et al., 1999; Pinkas et al., 2001). In order to obtain novel titanocene-ferrocene complexes, which to date are represented mostly by compounds having the metallocene units directly connected or separated by hydrocarbyl bridges (Štěpnička et al., 2000), we have studied the reactivity of Hdpf towards TiII complexes of the form [Ti(η5-C5R5)2(η2-Me3SiC≡CSiMe3)] (R is H or Me), which behave as a source of reactive titanocenes, [Ti(η5-C5R5)2] (Varga et al., 1996). The reaction of [Ti(η5-C5HMe4)2(η2-Me3SiC≡CSiMe3)] with one molar equivalent of Hdpf produced a novel paramagnetic titanocene-ferrocene complex, the title compound, (I), in high yield. \sch

The title complex has been characterized by spectral methods and its structure determined. The molecular structure is shown in Fig. 1 and selected geometric parameters are given in Table 1.

Both metallocene units exhibit the expected arrangement. The titanocene moiety is bent, with a dihedral angle of the least-squares cyclopentadienyl planes Cp3 and Cp4 of 46.24 (5)°, and is very nearly bisected by the TiO2 plane [angle between Cp3 and TiO2 22.88 (4), and angle between Cp4 and TiO2 23.46 (5)°]. The ring planes are defined as follows: Cp1 C1—C5, Cp2 C6—C10, Cp3 C30—C34, Cp4 C40—C44, Ph1 C12—C17, Ph2 C18—C23, TiO2 Ti/O1/O2 and CO2 C11/O1/O2. Please check carefully, as Cp and Ph rings were muddled in CIF. Cg denotes the ring centroid of the corresponding least-squares cyclopentadienyl plane. The Cg3—Ti—Cg4 angle is 137.09 (4)°, and the Ti—Cg distances differ only slightly: Ti—Cg3 2.0513 (8) and Ti—Cg4 2.0567 (8) Å. The titanocene cyclopentadienyls are staggered [τ(C30—Cg3—Cg4—C40) 39.1 (1)°; ideal value 36°], with the non-substituted ring C atoms located at the hinge position. The methyl substituents are disposed from the cyclopentadienyl planes towards the Ti centre, the maximum perpedicular distance being 0.100 (3) Å for atom C45 and the Cp4 plane.

The cyclopentadienyl rings of the bridging ferrocene unit are nearly parallel [Cp1/Cp2 1.1 (1)°] and, as indicated by the torsion angle τ(C1—Cg1—Cg2—C6) -163.4 (1)°, adopt a conformation half-way between anticlinal eclipsed (τ 144°) and antiperiplanar staggered (τ 180°). The distances of the Fe atom to the cyclopentadienyl ring centroids, Fe—Cg1 1.6513 (8) and Fe—Cg2 1.6476 (8) Å, correspond well to the Fe—Cg distances in uncoordinated Hdpf (Podlaha et al., 1995). Likewise, the arrangement at the phosphino substituent, which remains unaffected by coordination, resembles that of Hdpf [dihedral angles Ph1/Ph2 82.85 (5), Cp2/Ph1 75.31 (6) and Cp2/Ph2 84.06 (6)°].

The two metallocene units are mutually rotated, as defined by the dihedral angle of 24.93 (6)° between Cp1 and the TiO2 planes. Although the pseudotetrahedral arrangement around the Ti atom is severely distorted due to the steric requirements of the carboxylato and cyclopentadienyl ligands [O1—Ti—O2 60.85 (4) and Cg3—Ti—Cg4 46.24 (5)°], the carboxylato ligand is bonded in a symmetric fashion. The Ti—O bond lengths differ by only 0.014 Å, whilst the lengths of the carboxylic C—O bonds are identical within the precision of measurement. The four-membered ring Ti/O1/O2/C11 is slightly bent along the O1—O2 diagonal, with the carboxylic carbon C11 disposed by 0.124 (2) Å from the TiO2 plane, without, however, deformation of the planar arrangement at C11, as evidenced by the sum of the bond angles being 359.9°.

The arrangement of the carboxylato moiety is similar to the titanocene complex with chelating benzoate, [Ti(η5-C5H5)2(PhCO2-κ2O,O')] (Clauss et al., 1983), which exhibits Ti—O bond lengths of 2.134 (3), 2.147 (3), 2.152 (4) and 2.155 (3) Å (two independent molecules), and C—O distances in the range 1.254 (6)–1.271 (5) Å. As a comparison, the unidentate phosphinocarboxylate in [Ti(η5-C5H5)2(Ph2PCH2CO2-κO)2] (Edwards et al., 2000) shows similar Ti—O bond lengths of 1.925 (5) and 1.972 (4) Å, but clearly distinct C—O distances within the carboxylato moiety of 1.282 (8) and 1.300 (7) for C—O, and 1.189 (8) and 1.216 (6) Å for C═O.

The Cp1 and CO2 planes in (I) are rotated by as much as 19.3 (1)° from a coplanar arrangement and the C1—C11 bond is slightly shorter than the corresponding distance in Hdpf itself (1.452 and 1.458 Å). Nevertheless, it is likely that conjugation between the Cp1 ring and the carboxylato group remains active, since it has been shown for ferrocenoyl derivatives of the general formula [Fe(η5-C5H5)(η5-C5H4C(O)X)] (where X is OH or NH2) that the π-systems interact even at Cp-to-COX twist angles of 40–50° (Lin et al., 1998). Hence, the rotation as well as the bending of the Ti/O1/O2/C11 ring can be ascribed to inter- and intramolecular steric interactions of the bulky octamethyltitanocene and (diphenylphosphino)ferrocene moieties. An inspection of intermolecular contacts has revealed that solid-state packing is dictated mostly by steric requirements. The only notable exception is edge-to-face interaction between H21 and ferrocene cyclopentadienyl Cp1 in a neighbouring molecule [H21—Cg1i 2.845 Å, C21—Cg1i 3.708 (2) Å and C21—H21—Cg1i 155.0°; symmetry code: (i) x - 1, 1/2 - y, 1/2 + z].

Experimental top

On a vacuum line, a solution of Hdpf (207 mg, 0.50 mmol) in toluene (20 ml) was added to solid [Ti(η5-C5HMe4)2(η2-Me3SiC≡CSiMe3)] (235 mg, 0.51 mmol; Varga et al., 1996) and the resulting greenish-brown solution was heated to 333 K for 1 h. All volatiles were then removed under vacuum and the residue was extracted with hexane (50 ml). The extracts were concentrated to crystallization and kept at 273 K overnight to afford compound (I) as thin brown crystals. The mother liquor was concentrated and crystallized as above to provide an additional crop of crystals (combined yield: 307 mg, 84%; m.p. 398 K. Spectroscopic analysis: ESR (toluene, 295 K): g = 1.9793, H = 3.0 G, aTi = 7.3 G; IR (KBr, cm\-1): 3068 (w), 3050 (w), 2943 (m), 2907 (s), 2858 (m), 1585 (m), 1506 (s) [νas(CO2)], 1434 (m), 1396 (s) [νs(CO2)], 1358 (m), 1190 (w), 1163 (m), 1092 (w), 1027 (s), 828 (s), 812 (s), 798 (m), 744 (s), 697 (s), 634 (m), 506 (m), 486 (w), 451 (m), 422 (m); MS [m/z (relative abundance)]: 706 (6), 705 (21), 704 (53), 703 (100, M+), 702 (18), 701 (17), 582 (4), 352 (7), 305 (4), 292 (11), 290 (14), 289 {14, [(C5Me4H)2Ti - H]+}, 287 (4), 105 (7).

Refinement top

All H atoms were treated as riding with C—H = 0.96 Å (methyl) and 0.93 Å (aromatic).

Structure description top

Multidentate ligands possessing donor groups of different nature according to Pearson's HSAB concept (so-called hybrid ligands) Please define HSAB and provide a reference are capable of hemilabile coordination and of linking (different) transition metals into multinuclear complexes. Whereas the former property plays an important role in homogeneous catalysis, the latter is relevant mainly to fundamental research and material chemistry.

We have recently reported the synthesis of a ferrocene carboxyphosphine ligand, 1'-(diphenylphosphino)ferrocenecarboxylic acid (Hdpf; Podlaha et al., 1995), and its coordination properties towards various metals (Štěpnička et al., 1999; Pinkas et al., 2001). In order to obtain novel titanocene-ferrocene complexes, which to date are represented mostly by compounds having the metallocene units directly connected or separated by hydrocarbyl bridges (Štěpnička et al., 2000), we have studied the reactivity of Hdpf towards TiII complexes of the form [Ti(η5-C5R5)2(η2-Me3SiC≡CSiMe3)] (R is H or Me), which behave as a source of reactive titanocenes, [Ti(η5-C5R5)2] (Varga et al., 1996). The reaction of [Ti(η5-C5HMe4)2(η2-Me3SiC≡CSiMe3)] with one molar equivalent of Hdpf produced a novel paramagnetic titanocene-ferrocene complex, the title compound, (I), in high yield. \sch

The title complex has been characterized by spectral methods and its structure determined. The molecular structure is shown in Fig. 1 and selected geometric parameters are given in Table 1.

Both metallocene units exhibit the expected arrangement. The titanocene moiety is bent, with a dihedral angle of the least-squares cyclopentadienyl planes Cp3 and Cp4 of 46.24 (5)°, and is very nearly bisected by the TiO2 plane [angle between Cp3 and TiO2 22.88 (4), and angle between Cp4 and TiO2 23.46 (5)°]. The ring planes are defined as follows: Cp1 C1—C5, Cp2 C6—C10, Cp3 C30—C34, Cp4 C40—C44, Ph1 C12—C17, Ph2 C18—C23, TiO2 Ti/O1/O2 and CO2 C11/O1/O2. Please check carefully, as Cp and Ph rings were muddled in CIF. Cg denotes the ring centroid of the corresponding least-squares cyclopentadienyl plane. The Cg3—Ti—Cg4 angle is 137.09 (4)°, and the Ti—Cg distances differ only slightly: Ti—Cg3 2.0513 (8) and Ti—Cg4 2.0567 (8) Å. The titanocene cyclopentadienyls are staggered [τ(C30—Cg3—Cg4—C40) 39.1 (1)°; ideal value 36°], with the non-substituted ring C atoms located at the hinge position. The methyl substituents are disposed from the cyclopentadienyl planes towards the Ti centre, the maximum perpedicular distance being 0.100 (3) Å for atom C45 and the Cp4 plane.

The cyclopentadienyl rings of the bridging ferrocene unit are nearly parallel [Cp1/Cp2 1.1 (1)°] and, as indicated by the torsion angle τ(C1—Cg1—Cg2—C6) -163.4 (1)°, adopt a conformation half-way between anticlinal eclipsed (τ 144°) and antiperiplanar staggered (τ 180°). The distances of the Fe atom to the cyclopentadienyl ring centroids, Fe—Cg1 1.6513 (8) and Fe—Cg2 1.6476 (8) Å, correspond well to the Fe—Cg distances in uncoordinated Hdpf (Podlaha et al., 1995). Likewise, the arrangement at the phosphino substituent, which remains unaffected by coordination, resembles that of Hdpf [dihedral angles Ph1/Ph2 82.85 (5), Cp2/Ph1 75.31 (6) and Cp2/Ph2 84.06 (6)°].

The two metallocene units are mutually rotated, as defined by the dihedral angle of 24.93 (6)° between Cp1 and the TiO2 planes. Although the pseudotetrahedral arrangement around the Ti atom is severely distorted due to the steric requirements of the carboxylato and cyclopentadienyl ligands [O1—Ti—O2 60.85 (4) and Cg3—Ti—Cg4 46.24 (5)°], the carboxylato ligand is bonded in a symmetric fashion. The Ti—O bond lengths differ by only 0.014 Å, whilst the lengths of the carboxylic C—O bonds are identical within the precision of measurement. The four-membered ring Ti/O1/O2/C11 is slightly bent along the O1—O2 diagonal, with the carboxylic carbon C11 disposed by 0.124 (2) Å from the TiO2 plane, without, however, deformation of the planar arrangement at C11, as evidenced by the sum of the bond angles being 359.9°.

The arrangement of the carboxylato moiety is similar to the titanocene complex with chelating benzoate, [Ti(η5-C5H5)2(PhCO2-κ2O,O')] (Clauss et al., 1983), which exhibits Ti—O bond lengths of 2.134 (3), 2.147 (3), 2.152 (4) and 2.155 (3) Å (two independent molecules), and C—O distances in the range 1.254 (6)–1.271 (5) Å. As a comparison, the unidentate phosphinocarboxylate in [Ti(η5-C5H5)2(Ph2PCH2CO2-κO)2] (Edwards et al., 2000) shows similar Ti—O bond lengths of 1.925 (5) and 1.972 (4) Å, but clearly distinct C—O distances within the carboxylato moiety of 1.282 (8) and 1.300 (7) for C—O, and 1.189 (8) and 1.216 (6) Å for C═O.

The Cp1 and CO2 planes in (I) are rotated by as much as 19.3 (1)° from a coplanar arrangement and the C1—C11 bond is slightly shorter than the corresponding distance in Hdpf itself (1.452 and 1.458 Å). Nevertheless, it is likely that conjugation between the Cp1 ring and the carboxylato group remains active, since it has been shown for ferrocenoyl derivatives of the general formula [Fe(η5-C5H5)(η5-C5H4C(O)X)] (where X is OH or NH2) that the π-systems interact even at Cp-to-COX twist angles of 40–50° (Lin et al., 1998). Hence, the rotation as well as the bending of the Ti/O1/O2/C11 ring can be ascribed to inter- and intramolecular steric interactions of the bulky octamethyltitanocene and (diphenylphosphino)ferrocene moieties. An inspection of intermolecular contacts has revealed that solid-state packing is dictated mostly by steric requirements. The only notable exception is edge-to-face interaction between H21 and ferrocene cyclopentadienyl Cp1 in a neighbouring molecule [H21—Cg1i 2.845 Å, C21—Cg1i 3.708 (2) Å and C21—H21—Cg1i 155.0°; symmetry code: (i) x - 1, 1/2 - y, 1/2 + z].

Computing details top

Data collection: COLLECT (Nonius, 1997-2000); cell refinement: HKL SCALEPACK (Otwinowski & Minor 1997); data reduction: HKL DENZO (Otwinowski & Minor 1997) and SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 1999); software used to prepare material for publication: SHELXL97 and PLATON.

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of (I). Displacement ellipsoids are drawn at the 30% probability level. For clarity, H atoms have been omitted and only selected atoms within consecutively numbered rings are labelled.
µ-1κ2O,O':2(η5)-Cyclopentadienylcarboxylato- 2(η5)-diphenylphosphinocyclopentadienyl-bis[1,1(η5)- tetramethylcyclopentadienyl]iron(II)titanium(III) top
Crystal data top
[FeTi(C9H13)2(C6H4O2)(C17H14P)]F(000) = 1476
Mr = 703.48Dx = 1.337 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 8.4660 (1) ÅCell parameters from 97200 reflections
b = 29.5260 (3) Åθ = 1.0–27.5°
c = 14.1002 (1) ŵ = 0.72 mm−1
β = 97.3941 (5)°T = 150 K
V = 3495.28 (6) Å3Prism, dark red-brown
Z = 40.75 × 0.50 × 0.40 mm
Data collection top
Nonius KappaCCD area-detector
diffractometer		7976 independent reflections
Radiation source: fine-focus sealed tube6981 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.049
Detector resolution: 0.110 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω scansh = 0→10
Absorption correction: multi-scan
(SORTAV; Blessing, 1997)		k = −38→38
Tmin = 0.606, Tmax = 0.757l = −18→18
47188 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0368P)2 + 1.848P]
where P = (Fo2 + 2Fc2)/3
7976 reflections(Δ/σ)max = 0.001
415 parametersΔρmax = 0.29 e Å−3
0 restraintsΔρmin = −0.34 e Å−3
Crystal data top
[FeTi(C9H13)2(C6H4O2)(C17H14P)]V = 3495.28 (6) Å3
Mr = 703.48Z = 4
Monoclinic, P21/cMo Kα radiation
a = 8.4660 (1) ŵ = 0.72 mm−1
b = 29.5260 (3) ÅT = 150 K
c = 14.1002 (1) Å0.75 × 0.50 × 0.40 mm
β = 97.3941 (5)°
Data collection top
Nonius KappaCCD area-detector
diffractometer		7976 independent reflections
Absorption correction: multi-scan
(SORTAV; Blessing, 1997)		6981 reflections with I > 2σ(I)
Tmin = 0.606, Tmax = 0.757Rint = 0.049
47188 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0330 restraints
wR(F2) = 0.085H-atom parameters constrained
S = 1.04Δρmax = 0.29 e Å−3
7976 reflectionsΔρmin = −0.34 e Å−3
415 parameters
Special details top

Experimental. (rotation ω scans: 773 images, 0.7° ω rotation and 42 s exposure per frame)

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.

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

- 2.4680 (0.0111) x + 5.6535 (0.0659) y + 13.6339 (0.0092) z = 1.6613 (0.0065)

* 0.0000 (0.0000) C11 * 0.0000 (0.0000) O1 * 0.0000 (0.0000) O2 - 0.0914 (0.0055) C1

Rms deviation of fitted atoms = 0.0000

4.9673 (0.0059) x - 3.0939 (0.0247) y - 12.2926 (0.0059) z = 0.9130 (0.0070)

Angle to previous plane (with approximate e.s.d.) = 19.32 (0.12)

* 0.0004 (0.0010) C1 * 0.0012 (0.0010) C2 * -0.0024 (0.0011) C3 * 0.0026 (0.0011) C4 * -0.0019 (0.0010) C5 - 1.6512 (0.0008) Fe 0.0527 (0.0028) C11

Rms deviation of fitted atoms = 0.0019

- 5.0945 (0.0058) x + 2.8785 (0.0241) y + 12.1763 (0.0061) z = 2.2411 (0.0069)

Angle to previous plane (with approximate e.s.d.) = 1.12 (0.11)

* -0.0006 (0.0010) C6 * -0.0008 (0.0010) C7 * 0.0020 (0.0010) C8 * -0.0024 (0.0010) C9 * 0.0019 (0.0010) C10 - 1.6474 (0.0008) Fe -0.0096 (0.0027) P

Rms deviation of fitted atoms = 0.0017

- 1.7010 (0.0054) x + 0.7310 (0.0158) y + 14.0580 (0.0006) z = 1.8921 (0.0056)

Angle to previous plane (with approximate e.s.d.) = 25.89 (0.06)

* 0.0000 (0.0000) Ti * 0.0000 (0.0000) O1 * 0.0000 (0.0000) O2 - 0.1243 (0.0018) C11

Rms deviation of fitted atoms = 0.0000

0.2835 (0.0071) x - 8.6887 (0.0231) y + 13.2948 (0.0039) z = 5.1778 (0.0066)

Angle to previous plane (with approximate e.s.d.) = 22.88 (0.04)

* 0.0000 (0.0010) C30 * 0.0011 (0.0010) C31 * -0.0017 (0.0010) C32 * 0.0017 (0.0010) C33 * -0.0011 (0.0010) C34 - 2.0497 (0.0008) Ti 0.0295 (0.0030) C35 0.0661 (0.0030) C36 0.0443 (0.0031) C37 0.0956 (0.0030) C38

Rms deviation of fitted atoms = 0.0013

3.0973 (0.0065) x - 11.0436 (0.0228) y - 12.5802 (0.0053) z = 1.3445 (0.0070)

Angle to previous plane (with approximate e.s.d.) = 46.24 (0.05)

* 0.0084 (0.0010) C40 * -0.0078 (0.0010) C41 * 0.0043 (0.0010) C42 * 0.0009 (0.0010) C43 * -0.0057 (0.0010) C44 - 2.0531 (0.0008) Ti 0.1002 (0.0031) C45 0.0541 (0.0030) C46 0.0932 (0.0029) C47 0.0367 (0.0030) C48

Rms deviation of fitted atoms = 0.0061

- 1.7010 (0.0054) x + 0.7310 (0.0158) y + 14.0580 (0.0006) z = 1.8921 (0.0056)

Angle to previous plane (with approximate e.s.d.) = 23.46 (0.05)

* 0.0000 (0.0000) Ti * 0.0000 (0.0000) O1 * 0.0000 (0.0000) O2 - 0.1243 (0.0018) C11

Rms deviation of fitted atoms = 0.0000

4.9673 (0.0059) x - 3.0939 (0.0247) y - 12.2926 (0.0059) z = 0.9130 (0.0070)

Angle to previous plane (with approximate e.s.d.) = 24.93 (0.06)

* 0.0004 (0.0010) C1 * 0.0012 (0.0010) C2 * -0.0024 (0.0011) C3 * 0.0026 (0.0011) C4 * -0.0019 (0.0010) C5

Rms deviation of fitted atoms = 0.0019

- 6.5095 (0.0040) x + 16.3700 (0.0182) y - 3.0573 (0.0106) z = 2.3143 (0.0084)

Angle to previous plane (with approximate e.s.d.) = 75.31 (0.06)

* -0.0079 (0.0012) C12 * 0.0093 (0.0013) C13 * -0.0029 (0.0014) C14 * -0.0048 (0.0014) C15 * 0.0059 (0.0013) C16 * 0.0004 (0.0012) C17 - 0.0871 (0.0024) P

Rms deviation of fitted atoms = 0.0060

4.4462 (0.0054) x + 21.9239 (0.0157) y + 4.8602 (0.0101) z = 8.2932 (0.0045)

Angle to previous plane (with approximate e.s.d.) = 82.85 (0.05)

* -0.0001 (0.0012) C18 * -0.0030 (0.0013) C19 * 0.0042 (0.0014) C20 * -0.0024 (0.0014) C21 * -0.0006 (0.0014) C22 * 0.0019 (0.0013) C23 - 0.1516 (0.0025) P

Rms deviation of fitted atoms = 0.0025

4.9673 (0.0059) x - 3.0939 (0.0247) y - 12.2926 (0.0059) z = 0.9130 (0.0070)

Angle to previous plane (with approximate e.s.d.) = 84.06 (0.06)

* 0.0004 (0.0010) C1 * 0.0012 (0.0010) C2 * -0.0024 (0.0011) C3 * 0.0026 (0.0011) C4 * -0.0019 (0.0010) C5

Rms deviation of fitted atoms = 0.0019

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
xyzUiso*/Ueq
Fe0.57108 (3)0.204214 (7)0.239415 (16)0.02484 (7)
Ti0.95668 (3)0.050262 (10)0.247736 (19)0.02378 (8)
P0.24225 (5)0.273465 (14)0.21997 (3)0.02787 (10)
O10.95754 (13)0.12333 (4)0.24404 (8)0.0283 (2)
O20.73241 (13)0.08608 (4)0.21874 (8)0.0264 (2)
C10.72893 (19)0.16481 (5)0.17876 (11)0.0267 (3)
C20.7902 (2)0.20966 (6)0.19218 (13)0.0314 (4)
H20.88560.21780.22850.038*
C30.6805 (2)0.23970 (6)0.14057 (13)0.0372 (4)
H30.69110.27100.13740.045*
C40.5515 (2)0.21382 (6)0.09454 (13)0.0359 (4)
H40.46340.22520.05570.043*
C50.5800 (2)0.16741 (6)0.11812 (12)0.0312 (4)
H50.51390.14320.09780.037*
C60.38382 (19)0.23626 (5)0.28874 (12)0.0273 (3)
C70.3654 (2)0.18802 (6)0.29243 (12)0.0307 (3)
H70.28110.17140.26090.037*
C80.4981 (2)0.16998 (6)0.35243 (12)0.0325 (4)
H80.51540.13950.36720.039*
C90.5998 (2)0.20641 (6)0.38603 (12)0.0315 (4)
H90.69550.20400.42620.038*
C100.5298 (2)0.24711 (6)0.34747 (12)0.0288 (3)
H100.57170.27600.35850.035*
C110.80852 (19)0.12306 (5)0.21718 (11)0.0255 (3)
C120.36132 (19)0.32536 (6)0.21845 (13)0.0313 (4)
C130.4242 (2)0.33569 (7)0.13431 (15)0.0401 (4)
H130.39990.31730.08090.048*
C140.5220 (3)0.37288 (8)0.12909 (18)0.0519 (6)
H140.56460.37890.07280.062*
C150.5563 (2)0.40090 (7)0.2066 (2)0.0548 (6)
H150.62220.42590.20290.066*
C160.4929 (2)0.39200 (7)0.29052 (18)0.0484 (5)
H160.51510.41120.34270.058*
C170.3958 (2)0.35424 (6)0.29683 (14)0.0365 (4)
H170.35400.34830.35340.044*
C180.11076 (19)0.28714 (6)0.30973 (12)0.0280 (3)
C19−0.0129 (2)0.31774 (6)0.28428 (14)0.0353 (4)
H19−0.02120.33220.22520.042*
C20−0.1239 (2)0.32684 (7)0.34622 (15)0.0419 (4)
H20−0.20500.34760.32870.050*
C21−0.1147 (2)0.30530 (7)0.43359 (14)0.0392 (4)
H21−0.18990.31120.47460.047*
C220.0070 (2)0.27491 (7)0.45975 (14)0.0394 (4)
H220.01410.26040.51870.047*
C230.1191 (2)0.26594 (6)0.39823 (13)0.0353 (4)
H230.20070.24540.41660.042*
C301.1007 (2)0.00824 (6)0.37137 (11)0.0299 (3)
H301.1903−0.00780.35900.036*
C311.10027 (19)0.05370 (6)0.40117 (11)0.0290 (3)
C320.9399 (2)0.06473 (6)0.41159 (11)0.0301 (3)
C330.8447 (2)0.02570 (6)0.38837 (12)0.0317 (4)
C340.9437 (2)−0.00937 (6)0.36313 (12)0.0316 (4)
C351.2422 (2)0.08408 (7)0.42014 (14)0.0399 (4)
H35A1.27360.08640.48790.048*
H35B1.21570.11360.39440.048*
H35C1.32850.07180.39030.048*
C360.8814 (2)0.10879 (7)0.44673 (13)0.0422 (4)
H36A0.78540.11760.40720.051*
H36B0.96120.13170.44390.051*
H36C0.86020.10530.51160.051*
C370.6686 (2)0.02262 (8)0.39332 (14)0.0458 (5)
H37A0.6281−0.00510.36420.055*
H37B0.61560.04780.35990.055*
H37C0.64960.02320.45900.055*
C380.8952 (3)−0.05746 (7)0.34001 (14)0.0444 (5)
H38A0.8926−0.07410.39830.053*
H38B0.9706−0.07120.30350.053*
H38C0.7914−0.05780.30350.053*
C401.0551 (2)−0.00696 (6)0.15835 (12)0.0310 (4)
H401.0843−0.03430.18820.037*
C411.1577 (2)0.03072 (6)0.15180 (12)0.0313 (4)
C421.0674 (2)0.06464 (6)0.09884 (11)0.0303 (3)
C430.9105 (2)0.04824 (6)0.07489 (11)0.0284 (3)
C440.9014 (2)0.00394 (6)0.11205 (11)0.0294 (3)
C451.3338 (2)0.03217 (8)0.18530 (14)0.0438 (5)
H45A1.39150.02570.13260.053*
H45B1.35980.01000.23460.053*
H45C1.36240.06170.21010.053*
C461.1289 (2)0.10963 (7)0.07051 (13)0.0391 (4)
H46A1.12510.11090.00220.047*
H46B1.23690.11340.09970.047*
H46C1.06400.13340.09140.047*
C470.7770 (2)0.07199 (6)0.01381 (12)0.0361 (4)
H47A0.77410.0623−0.05140.043*
H47B0.79400.10410.01750.043*
H47C0.67770.06480.03630.043*
C480.7570 (2)−0.02593 (7)0.09934 (13)0.0390 (4)
H48A0.6735−0.01210.12940.047*
H48B0.7831−0.05490.12820.047*
H48C0.7219−0.02990.03240.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe0.02460 (12)0.02365 (12)0.02713 (12)0.00319 (8)0.00659 (9)−0.00018 (9)
Ti0.02200 (14)0.02672 (15)0.02231 (14)0.00377 (10)0.00171 (10)0.00053 (11)
P0.0247 (2)0.0295 (2)0.0292 (2)0.00203 (16)0.00268 (16)−0.00304 (17)
O10.0243 (6)0.0290 (6)0.0315 (6)0.0020 (4)0.0028 (5)−0.0015 (5)
O20.0236 (5)0.0271 (6)0.0283 (6)0.0025 (4)0.0031 (4)0.0002 (4)
C10.0266 (8)0.0284 (8)0.0264 (8)0.0049 (6)0.0087 (6)−0.0005 (6)
C20.0277 (8)0.0300 (8)0.0385 (9)0.0013 (6)0.0122 (7)0.0020 (7)
C30.0425 (10)0.0307 (9)0.0420 (10)0.0065 (7)0.0201 (8)0.0091 (8)
C40.0393 (10)0.0416 (10)0.0284 (8)0.0145 (8)0.0101 (7)0.0069 (7)
C50.0310 (9)0.0361 (9)0.0269 (8)0.0069 (7)0.0047 (7)−0.0036 (7)
C60.0248 (8)0.0285 (8)0.0297 (8)0.0025 (6)0.0080 (6)−0.0034 (6)
C70.0285 (8)0.0293 (8)0.0358 (9)−0.0014 (7)0.0100 (7)−0.0026 (7)
C80.0352 (9)0.0306 (9)0.0337 (9)0.0044 (7)0.0125 (7)0.0057 (7)
C90.0300 (9)0.0377 (9)0.0273 (8)0.0064 (7)0.0055 (7)−0.0003 (7)
C100.0281 (8)0.0292 (8)0.0292 (8)0.0033 (6)0.0043 (6)−0.0056 (7)
C110.0267 (8)0.0284 (8)0.0222 (7)0.0028 (6)0.0064 (6)−0.0025 (6)
C120.0247 (8)0.0285 (8)0.0403 (9)0.0061 (6)0.0022 (7)0.0039 (7)
C130.0350 (10)0.0412 (10)0.0442 (10)0.0068 (8)0.0053 (8)0.0107 (8)
C140.0398 (11)0.0486 (12)0.0681 (15)0.0041 (9)0.0093 (10)0.0269 (11)
C150.0313 (10)0.0357 (11)0.0952 (19)0.0015 (8)0.0004 (11)0.0234 (12)
C160.0323 (10)0.0312 (10)0.0776 (15)0.0054 (8)−0.0091 (10)−0.0073 (10)
C170.0280 (9)0.0321 (9)0.0483 (11)0.0050 (7)0.0007 (8)−0.0034 (8)
C180.0225 (8)0.0288 (8)0.0325 (8)−0.0003 (6)0.0023 (6)−0.0046 (7)
C190.0288 (9)0.0359 (9)0.0409 (10)0.0055 (7)0.0033 (7)0.0023 (8)
C200.0274 (9)0.0416 (10)0.0567 (12)0.0092 (7)0.0053 (8)−0.0052 (9)
C210.0281 (9)0.0446 (10)0.0463 (11)−0.0007 (8)0.0108 (8)−0.0115 (9)
C220.0372 (10)0.0471 (11)0.0349 (9)0.0034 (8)0.0081 (8)−0.0028 (8)
C230.0287 (9)0.0415 (10)0.0356 (9)0.0071 (7)0.0031 (7)0.0001 (8)
C300.0284 (8)0.0360 (9)0.0247 (8)0.0065 (7)0.0006 (6)0.0049 (7)
C310.0257 (8)0.0375 (9)0.0229 (7)0.0011 (7)−0.0006 (6)0.0019 (7)
C320.0274 (8)0.0401 (9)0.0223 (7)0.0057 (7)0.0014 (6)0.0013 (7)
C330.0258 (8)0.0456 (10)0.0231 (8)−0.0014 (7)0.0007 (6)0.0070 (7)
C340.0340 (9)0.0363 (9)0.0231 (8)−0.0013 (7)−0.0015 (7)0.0060 (7)
C350.0317 (9)0.0497 (11)0.0370 (10)−0.0077 (8)−0.0003 (8)−0.0004 (8)
C360.0445 (11)0.0519 (12)0.0301 (9)0.0147 (9)0.0042 (8)−0.0041 (8)
C370.0275 (9)0.0709 (14)0.0389 (10)−0.0023 (9)0.0039 (8)0.0127 (10)
C380.0575 (13)0.0387 (10)0.0349 (10)−0.0095 (9)−0.0018 (9)0.0076 (8)
C400.0359 (9)0.0317 (8)0.0258 (8)0.0106 (7)0.0056 (7)0.0009 (7)
C410.0272 (8)0.0409 (10)0.0264 (8)0.0075 (7)0.0056 (6)0.0003 (7)
C420.0323 (9)0.0354 (9)0.0239 (8)0.0053 (7)0.0064 (6)0.0005 (7)
C430.0301 (8)0.0333 (9)0.0218 (7)0.0078 (7)0.0038 (6)−0.0019 (6)
C440.0319 (9)0.0321 (8)0.0244 (8)0.0039 (7)0.0045 (6)−0.0046 (6)
C450.0283 (9)0.0670 (14)0.0362 (10)0.0090 (9)0.0050 (8)0.0041 (9)
C460.0411 (10)0.0424 (10)0.0349 (9)−0.0012 (8)0.0086 (8)0.0043 (8)
C470.0384 (10)0.0434 (10)0.0254 (8)0.0126 (8)−0.0004 (7)−0.0021 (7)
C480.0417 (10)0.0404 (10)0.0344 (9)−0.0040 (8)0.0027 (8)−0.0064 (8)
Geometric parameters (Å, º) top
Fe—C12.0409 (15)C17—H170.9300
Fe—C22.0566 (17)C18—C231.390 (2)
Fe—C32.0569 (17)C18—C191.395 (2)
Fe—C42.0478 (17)C19—C201.389 (3)
Fe—C52.0360 (17)C19—H190.9300
Fe—C62.0435 (16)C20—C211.380 (3)
Fe—C72.0380 (17)C20—H200.9300
Fe—C82.0484 (17)C21—C221.380 (3)
Fe—C92.0512 (17)C21—H210.9300
Fe—C102.0457 (16)C22—C231.391 (3)
Ti—O12.1582 (12)C22—H220.9300
Ti—O22.1658 (11)C23—H230.9300
Ti—C302.3489 (16)C30—C311.407 (2)
Ti—C312.3435 (16)C30—C341.418 (2)
Ti—C322.3718 (16)C30—H300.9300
Ti—C332.4166 (16)C31—C321.422 (2)
Ti—C342.4095 (17)C31—C351.496 (2)
Ti—C402.3256 (16)C32—C331.420 (3)
Ti—C412.3771 (16)C32—C361.498 (2)
Ti—C422.4440 (16)C33—C341.406 (3)
Ti—C432.4189 (16)C33—C371.505 (2)
Ti—C442.3493 (16)C34—C381.502 (3)
P—C61.8122 (17)C35—H35A0.9600
P—C121.8359 (18)C35—H35B0.9600
P—C181.8349 (17)C35—H35C0.9600
O1—C111.2697 (19)C36—H36A0.9600
O2—C111.2693 (19)C36—H36B0.9600
C1—C21.426 (2)C36—H36C0.9600
C1—C51.431 (2)C37—H37A0.9600
C1—C111.474 (2)C37—H37B0.9600
C2—C31.416 (3)C37—H37C0.9600
C2—H20.9300C38—H38A0.9600
C3—C41.420 (3)C38—H38B0.9600
C3—H30.9300C38—H38C0.9600
C4—C51.423 (2)C40—C441.416 (2)
C4—H40.9300C40—C411.421 (3)
C5—H50.9300C40—H400.9300
C6—C101.433 (2)C41—C421.413 (2)
C6—C71.434 (2)C41—C451.506 (2)
C7—C81.420 (3)C42—C431.413 (2)
C7—H70.9300C42—C461.500 (3)
C8—C91.421 (3)C43—C441.415 (2)
C8—H80.9300C43—C471.504 (2)
C9—C101.417 (2)C44—C481.500 (2)
C9—H90.9300C45—H45A0.9600
C10—H100.9300C45—H45B0.9600
C12—C131.395 (3)C45—H45C0.9600
C12—C171.397 (3)C46—H46A0.9600
C13—C141.383 (3)C46—H46B0.9600
C13—H130.9300C46—H46C0.9600
C14—C151.372 (4)C47—H47A0.9600
C14—H140.9300C47—H47B0.9600
C15—C161.386 (3)C47—H47C0.9600
C15—H150.9300C48—H48A0.9600
C16—C171.394 (3)C48—H48B0.9600
C16—H160.9300C48—H48C0.9600
O1—Ti—O260.85 (4)C34—C30—H30125.2
C6—P—C12100.71 (8)C30—C31—C32106.76 (15)
C6—P—C18100.52 (8)C30—C31—C35126.36 (16)
C12—P—C18101.96 (8)C32—C31—C35126.87 (16)
C11—O1—Ti89.68 (9)C33—C32—C31108.12 (15)
C11—O2—Ti89.35 (9)C33—C32—C36125.39 (16)
C2—C1—C5107.87 (15)C31—C32—C36126.39 (17)
C2—C1—C11125.91 (15)C34—C33—C32108.50 (15)
C5—C1—C11126.17 (15)C34—C33—C37126.40 (18)
C3—C2—C1108.06 (16)C32—C33—C37125.07 (17)
C3—C2—H2126.0C33—C34—C30106.96 (15)
C1—C2—H2126.0C33—C34—C38126.58 (17)
C2—C3—C4108.24 (16)C30—C34—C38126.28 (17)
C2—C3—H3125.9C31—C35—H35A109.5
C4—C3—H3125.9C31—C35—H35B109.5
C3—C4—C5108.30 (16)H35A—C35—H35B109.5
C3—C4—H4125.8C31—C35—H35C109.5
C5—C4—H4125.8H35A—C35—H35C109.5
C4—C5—C1107.52 (16)H35B—C35—H35C109.5
C4—C5—H5126.2C32—C36—H36A109.5
C1—C5—H5126.2C32—C36—H36B109.5
C10—C6—C7106.90 (14)H36A—C36—H36B109.5
C10—C6—P129.47 (13)C32—C36—H36C109.5
C7—C6—P123.63 (13)H36A—C36—H36C109.5
C8—C7—C6108.23 (15)H36B—C36—H36C109.5
C8—C7—H7125.9C33—C37—H37A109.5
C6—C7—H7125.9C33—C37—H37B109.5
C7—C8—C9108.29 (15)H37A—C37—H37B109.5
C7—C8—H8125.9C33—C37—H37C109.5
C9—C8—H8125.9H37A—C37—H37C109.5
C10—C9—C8107.97 (15)H37B—C37—H37C109.5
C10—C9—H9126.0C34—C38—H38A109.5
C8—C9—H9126.0C34—C38—H38B109.5
C9—C10—C6108.61 (15)H38A—C38—H38B109.5
C9—C10—H10125.7C34—C38—H38C109.5
C6—C10—H10125.7H38A—C38—H38C109.5
O2—C11—O1119.18 (14)H38B—C38—H38C109.5
O2—C11—C1121.10 (14)C44—C40—C41108.95 (15)
O1—C11—C1119.59 (14)C44—C40—H40125.5
C13—C12—C17118.40 (17)C41—C40—H40125.5
C13—C12—P117.55 (14)Ti—C40—H40118.6
C17—C12—P124.02 (14)C42—C41—C40107.21 (15)
C14—C13—C12121.0 (2)C42—C41—C45126.29 (17)
C14—C13—H13119.5C40—C41—C45126.18 (16)
C12—C13—H13119.5C43—C42—C41108.12 (15)
C15—C14—C13120.2 (2)C43—C42—C46125.98 (16)
C15—C14—H14119.9C41—C42—C46125.87 (16)
C13—C14—H14119.9C42—C43—C44108.82 (14)
C14—C15—C16120.0 (2)C42—C43—C47126.25 (16)
C14—C15—H15120.0C44—C43—C47124.78 (16)
C16—C15—H15120.0C43—C44—C40106.87 (15)
C15—C16—C17120.2 (2)C43—C44—C48125.59 (16)
C15—C16—H16119.9C40—C44—C48127.47 (16)
C17—C16—H16119.9C41—C45—H45A109.5
C16—C17—C12120.17 (19)C41—C45—H45B109.5
C16—C17—H17119.9H45A—C45—H45B109.5
C12—C17—H17119.9C41—C45—H45C109.5
C23—C18—C19118.20 (16)H45A—C45—H45C109.5
C23—C18—P123.72 (13)H45B—C45—H45C109.5
C19—C18—P117.85 (13)C42—C46—H46A109.5
C20—C19—C18120.65 (18)C42—C46—H46B109.5
C20—C19—H19119.7H46A—C46—H46B109.5
C18—C19—H19119.7C42—C46—H46C109.5
C21—C20—C19120.47 (17)H46A—C46—H46C109.5
C21—C20—H20119.8H46B—C46—H46C109.5
C19—C20—H20119.8C43—C47—H47A109.5
C20—C21—C22119.54 (17)C43—C47—H47B109.5
C20—C21—H21120.2H47A—C47—H47B109.5
C22—C21—H21120.2C43—C47—H47C109.5
C21—C22—C23120.18 (18)H47A—C47—H47C109.5
C21—C22—H22119.9H47B—C47—H47C109.5
C23—C22—H22119.9C44—C48—H48A109.5
C18—C23—C22120.96 (17)C44—C48—H48B109.5
C18—C23—H23119.5H48A—C48—H48B109.5
C22—C23—H23119.5C44—C48—H48C109.5
C31—C30—C34109.65 (15)H48A—C48—H48C109.5
C31—C30—H30125.2H48B—C48—H48C109.5
O1—Ti—O2—C115.62 (8)P—C12—C17—C16177.31 (13)
C5—C1—C2—C30.07 (18)C6—P—C18—C23−8.74 (17)
C11—C1—C2—C3177.63 (15)C12—P—C18—C23−112.18 (16)
C1—C2—C3—C4−0.34 (19)C6—P—C18—C19176.97 (14)
C2—C3—C4—C50.5 (2)C12—P—C18—C1973.53 (15)
C3—C4—C5—C1−0.43 (19)C23—C18—C19—C200.4 (3)
C2—C1—C5—C40.22 (18)P—C18—C19—C20174.99 (15)
C11—C1—C5—C4−177.33 (15)C18—C19—C20—C21−0.8 (3)
C18—P—C6—C10−89.32 (16)C19—C20—C21—C220.7 (3)
C12—P—C6—C1015.14 (17)C20—C21—C22—C23−0.3 (3)
C18—P—C6—C790.99 (14)C19—C18—C23—C220.1 (3)
C12—P—C6—C7−164.56 (14)P—C18—C23—C22−174.19 (14)
C10—C6—C7—C80.02 (18)C21—C22—C23—C18−0.1 (3)
P—C6—C7—C8179.78 (12)C34—C30—C31—C35178.71 (16)
C6—C7—C8—C9−0.27 (19)C30—C31—C32—C330.26 (18)
C7—C8—C9—C100.42 (19)C35—C31—C32—C33−178.54 (16)
C8—C9—C10—C6−0.41 (19)C30—C31—C32—C36176.77 (16)
C7—C6—C10—C90.24 (18)C35—C31—C32—C36−2.0 (3)
P—C6—C10—C9−179.50 (12)C31—C32—C33—C34−0.33 (18)
Ti—O2—C11—O1−9.59 (14)C36—C32—C33—C34−176.89 (16)
Ti—O1—C11—C1−166.29 (13)C31—C32—C33—C37177.95 (16)
Ti—O2—C11—C1166.26 (13)C36—C32—C33—C371.4 (3)
Ti—O1—C11—O29.62 (14)C32—C33—C34—C300.27 (18)
C2—C1—C11—O2165.14 (15)C37—C33—C34—C30−177.99 (16)
C2—C1—C11—O1−19.0 (2)C32—C33—C34—C38175.50 (16)
C5—C1—C11—O2−17.7 (2)C37—C33—C34—C38−2.8 (3)
C5—C1—C11—O1158.10 (15)C31—C30—C34—C33−0.10 (19)
C2—C1—C11—Ti−102.5 (6)C31—C30—C34—C38−175.36 (16)
C5—C1—C11—Ti74.6 (6)C44—C40—C41—C42−1.55 (18)
O1—Ti—C11—O2−170.31 (14)C44—C40—C41—C45−175.25 (16)
O2—Ti—C11—O1170.31 (14)C40—C41—C42—C431.14 (18)
O1—Ti—C11—C190.4 (6)C45—C41—C42—C43174.84 (16)
O2—Ti—C11—C1−99.3 (6)C40—C41—C42—C46−177.17 (16)
C6—P—C12—C13103.49 (14)C45—C41—C42—C46−3.5 (3)
C18—P—C12—C13−153.22 (13)C41—C42—C43—C44−0.33 (18)
C6—P—C12—C17−74.77 (15)C46—C42—C43—C44177.98 (16)
C18—P—C12—C1728.53 (16)C41—C42—C43—C47−176.09 (15)
C17—C12—C13—C141.8 (3)C46—C42—C43—C472.2 (3)
P—C12—C13—C14−176.57 (15)C42—C43—C44—C40−0.62 (18)
C12—C13—C14—C15−1.3 (3)C47—C43—C44—C40175.22 (15)
C13—C14—C15—C160.0 (3)C42—C43—C44—C48−177.76 (15)
C14—C15—C16—C170.9 (3)C47—C43—C44—C48−1.9 (3)
C15—C16—C17—C12−0.4 (3)C41—C40—C44—C431.34 (18)
C13—C12—C17—C16−0.9 (3)C41—C40—C44—C48178.41 (16)

Experimental details

Crystal data
Chemical formula[FeTi(C9H13)2(C6H4O2)(C17H14P)]
Mr703.48
Crystal system, space groupMonoclinic, P21/c
Temperature (K)150
a, b, c (Å)8.4660 (1), 29.5260 (3), 14.1002 (1)
β (°) 97.3941 (5)
V (Å3)3495.28 (6)
Z4
Radiation typeMo Kα
µ (mm−1)0.72
Crystal size (mm)0.75 × 0.50 × 0.40
Data collection
DiffractometerNonius KappaCCD area-detector
Absorption correctionMulti-scan
(SORTAV; Blessing, 1997)
Tmin, Tmax0.606, 0.757
No. of measured, independent and
observed [I > 2σ(I)] reflections		47188, 7976, 6981
Rint0.049
(sin θ/λ)max (Å−1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.085, 1.04
No. of reflections7976
No. of parameters415
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)0.29, −0.34

Computer programs: COLLECT (Nonius, 1997-2000), HKL SCALEPACK (Otwinowski & Minor 1997), HKL DENZO (Otwinowski & Minor 1997) and SCALEPACK, SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), PLATON (Spek, 1999), SHELXL97 and PLATON.

Selected geometric parameters (Å, º) top
Fe—C12.0409 (15)Ti—C322.3718 (16)
Fe—C22.0566 (17)Ti—C332.4166 (16)
Fe—C32.0569 (17)Ti—C342.4095 (17)
Fe—C42.0478 (17)Ti—C402.3256 (16)
Fe—C52.0360 (17)Ti—C412.3771 (16)
Fe—C62.0435 (16)Ti—C422.4440 (16)
Fe—C72.0380 (17)Ti—C432.4189 (16)
Fe—C82.0484 (17)Ti—C442.3493 (16)
Fe—C92.0512 (17)P—C61.8122 (17)
Fe—C102.0457 (16)P—C121.8359 (18)
Ti—O12.1582 (12)P—C181.8349 (17)
Ti—O22.1658 (11)O1—C111.2697 (19)
Ti—C302.3489 (16)O2—C111.2693 (19)
Ti—C312.3435 (16)C1—C111.474 (2)
O1—Ti—O260.85 (4)C11—O2—Ti89.35 (9)
C6—P—C12100.71 (8)O2—C11—O1119.18 (14)
C6—P—C18100.52 (8)O2—C11—C1121.10 (14)
C12—P—C18101.96 (8)O1—C11—C1119.59 (14)
C11—O1—Ti89.68 (9)
Ti—O1—C11—C1−166.29 (13)C2—C1—C11—O1−19.0 (2)
Ti—O2—C11—C1166.26 (13)C5—C1—C11—O2−17.7 (2)
 

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