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The structure of a pincer ligand consists of a backbone and two `arms' which typically contain a P or N atom. They are tridentate ligands that coordinate to a metal center in a meridional configuration. A series of three iron complexes containing the pyrrole-based PNP pincer ligand 2,5-bis­[(diisoprop­ylphosphan­yl)meth­yl]pyrrolide (PNpyrP) has been synthesized. These complexes are possible precursors to new iron catalysts. {2,5-Bis[(diisoprop­ylphosphan­yl)meth­yl]pyrrolido-κ3P,N,P′}carbonyl­chlorido­(tri­methyl­phosphane-κP)iron(II), [Fe(C18H34NP2)Cl(C3H9P)(CO)] or [Fe(PNpyrP)Cl(PMe3)(CO)], (I), has a slightly distorted octa­hedral geometry, with the Cl and CO ligands occupying the apical positions. {2,5-Bis[(diisoprop­ylphosphan­yl)meth­yl]pyrrolido-κ3P,N,P′}chlorido­(pyridine-κN)iron(II), [Fe(C18H34NP2)Cl(C5H5N)] or [Fe(PNpyrP)Cl(py)] (py is pyridine), (II), is a five-coordinate square-pyramidal complex, with the pyridine ligand in the apical position. {2,5-Bis[(diisoprop­ylphosphan­yl)meth­yl]pyrrolido-κ3P,N,P′}di­carbonyl­chlorido­iron(II), [Fe(C18H34NP2)Cl(CO)2] or [Fe(PNpyrP)Cl(CO)2], (III), is structurally similar to (I), but with the PMe3 ligand replaced by a second carbonyl ligand from the reaction of (II) with CO. The two carbonyl ligands are in a cis configuration, and there is positional disorder of the chloride and trans carbonyl ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617009287/ky3121sup1.cif
Contains datablocks global, I, II, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617009287/ky3121Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617009287/ky3121IIsup3.hkl
Contains datablock II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617009287/ky3121IIIsup4.hkl
Contains datablock III

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2053229617009287/ky3121sup5.pdf
NMR spectra

CCDC references: 1557265; 1557264; 1557263

Computing details top

For all compounds, data collection: SAINT (Bruker, 2015); cell refinement: SAINT (Bruker, 2015); data reduction: SAINT (Bruker, 2015). Program(s) used to solve structure: SHELXT (Sheldrick, 2015a) for (I), (III); olex2.solve (Bourhis et al., 2015) for (II). Program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b) for (I), (III); SHELXL2016 (Sheldrick, 2015b) for (II). For all compounds, molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

(I) {2,5-Bis[(diisopropylphosphanyl)methyl]pyrrolido-κ3P,N,P'}carbonylchlorido(trimethylphosphane-κP)iron(II) top
Crystal data top
[Fe(C18H34NP2)Cl(C3H9P)(CO)]F(000) = 1112
Mr = 521.78Dx = 1.356 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 17.0243 (16) ÅCell parameters from 9059 reflections
b = 10.494 (1) Åθ = 2.3–27.9°
c = 15.1374 (14) ŵ = 0.90 mm1
β = 109.090 (3)°T = 120 K
V = 2555.6 (4) Å3Rod, orange
Z = 40.44 × 0.15 × 0.09 mm
Data collection top
Bruker APEXII CCD
diffractometer
6421 independent reflections
Radiation source: fine-focus sealed tube5417 reflections with I > 2σ(I)
Detector resolution: 8.33 pixels mm-1Rint = 0.049
φ and ω scansθmax = 28.5°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
h = 2222
Tmin = 0.664, Tmax = 0.746k = 1413
65628 measured reflectionsl = 1920
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.030P)2 + 2.290P]
where P = (Fo2 + 2Fc2)/3
6421 reflections(Δ/σ)max = 0.001
273 parametersΔρmax = 0.69 e Å3
0 restraintsΔρmin = 0.40 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.74275 (2)0.48764 (2)0.87576 (2)0.01299 (6)
Cl10.66509 (3)0.37458 (4)0.73868 (3)0.02033 (10)
P10.82669 (3)0.59346 (4)0.80510 (3)0.01412 (9)
P20.70737 (3)0.32606 (4)0.95927 (3)0.01529 (10)
P30.62985 (3)0.61581 (4)0.83773 (3)0.01965 (10)
O10.82605 (9)0.62872 (13)1.04304 (9)0.0256 (3)
N10.83671 (9)0.36830 (13)0.89447 (10)0.0145 (3)
C10.91419 (11)0.39862 (17)0.89198 (12)0.0162 (3)
C20.83528 (11)0.24005 (16)0.91080 (12)0.0174 (3)
C30.91175 (12)0.18785 (17)0.91757 (13)0.0201 (4)
H30.92750.10090.92860.024*
C40.96197 (11)0.28952 (17)0.90484 (12)0.0191 (4)
H41.01770.28370.90510.023*
C50.92901 (11)0.53630 (17)0.87792 (13)0.0182 (3)
H5A0.97060.54680.84560.022*
H5B0.94830.58220.93830.022*
C60.75766 (11)0.18961 (16)0.92251 (13)0.0189 (4)
H6A0.77060.12180.97060.023*
H6B0.72070.15390.86290.023*
C70.81768 (12)0.53001 (17)0.68775 (12)0.0197 (4)
H70.79960.43930.68770.024*
C80.89772 (15)0.5257 (2)0.66308 (17)0.0379 (6)
H8A0.91860.61250.66200.057*
H8B0.88650.48650.60140.057*
H8C0.93950.47530.71000.057*
C90.74841 (15)0.5959 (2)0.61168 (14)0.0322 (5)
H9A0.69620.58780.62530.048*
H9B0.74230.55610.55120.048*
H9C0.76200.68630.60940.048*
C100.83630 (12)0.76974 (16)0.79928 (13)0.0198 (4)
H100.78940.79960.74400.024*
C110.91649 (14)0.81490 (19)0.78530 (16)0.0309 (5)
H11A0.96420.78580.83770.046*
H11B0.91670.90820.78240.046*
H11C0.92020.77970.72680.046*
C120.82722 (13)0.83620 (17)0.88490 (14)0.0254 (4)
H12A0.77580.80790.89460.038*
H12B0.82520.92860.87520.038*
H12C0.87480.81480.94000.038*
C130.59921 (11)0.26886 (17)0.93367 (13)0.0197 (4)
H130.57070.27890.86490.024*
C140.59263 (14)0.1279 (2)0.95694 (16)0.0326 (5)
H14A0.61870.07540.92070.049*
H14B0.53390.10420.94120.049*
H14C0.62100.11391.02380.049*
C150.54999 (13)0.3469 (2)0.98283 (16)0.0344 (5)
H15A0.56560.32071.04840.052*
H15B0.49040.33250.95210.052*
H15C0.56240.43760.97950.052*
C160.75262 (12)0.32256 (18)1.08894 (13)0.0213 (4)
H160.73290.24171.10960.026*
C170.84810 (13)0.3160 (2)1.12313 (14)0.0281 (4)
H17A0.86600.24501.09220.042*
H17B0.86860.30281.19090.042*
H17C0.87060.39601.10800.042*
C180.72538 (14)0.4310 (2)1.14050 (14)0.0288 (4)
H18A0.74040.51311.11960.043*
H18B0.75330.42191.20800.043*
H18C0.66500.42731.12680.043*
C190.61832 (13)0.7339 (2)0.74540 (16)0.0319 (5)
H19A0.66570.79250.76400.048*
H19B0.56680.78200.73540.048*
H19C0.61630.69050.68740.048*
C200.61926 (13)0.7175 (2)0.93058 (16)0.0304 (5)
H20A0.61970.66490.98420.046*
H20B0.56670.76450.90790.046*
H20C0.66560.77800.94970.046*
C210.52587 (12)0.5462 (2)0.79256 (15)0.0280 (4)
H21A0.51980.50130.73400.042*
H21B0.48410.61400.78110.042*
H21C0.51790.48610.83840.042*
C220.79219 (11)0.57246 (16)0.97588 (13)0.0180 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01322 (12)0.01225 (12)0.01398 (12)0.00068 (9)0.00509 (9)0.00120 (9)
Cl10.0194 (2)0.0220 (2)0.0187 (2)0.00379 (17)0.00517 (17)0.00460 (16)
P10.0146 (2)0.01292 (19)0.0147 (2)0.00178 (16)0.00475 (17)0.00015 (16)
P20.0159 (2)0.0147 (2)0.0168 (2)0.00039 (16)0.00738 (17)0.00058 (16)
P30.0166 (2)0.0187 (2)0.0223 (2)0.00013 (17)0.00443 (19)0.00075 (18)
O10.0305 (8)0.0256 (7)0.0200 (7)0.0071 (6)0.0074 (6)0.0067 (6)
N10.0141 (7)0.0149 (7)0.0151 (7)0.0006 (5)0.0055 (6)0.0004 (5)
C10.0142 (8)0.0193 (8)0.0142 (8)0.0007 (6)0.0034 (6)0.0005 (6)
C20.0194 (9)0.0148 (8)0.0187 (9)0.0005 (7)0.0072 (7)0.0011 (6)
C30.0217 (9)0.0168 (8)0.0210 (9)0.0042 (7)0.0060 (7)0.0013 (7)
C40.0144 (8)0.0237 (9)0.0187 (9)0.0019 (7)0.0050 (7)0.0022 (7)
C50.0132 (8)0.0210 (9)0.0191 (9)0.0017 (7)0.0035 (7)0.0008 (7)
C60.0215 (9)0.0131 (8)0.0241 (9)0.0001 (7)0.0101 (7)0.0009 (7)
C70.0248 (9)0.0181 (8)0.0172 (9)0.0052 (7)0.0084 (7)0.0013 (7)
C80.0405 (13)0.0449 (13)0.0389 (13)0.0155 (11)0.0272 (11)0.0180 (10)
C90.0469 (13)0.0274 (10)0.0182 (10)0.0007 (9)0.0051 (9)0.0008 (8)
C100.0216 (9)0.0140 (8)0.0230 (9)0.0028 (7)0.0061 (7)0.0012 (7)
C110.0354 (12)0.0208 (9)0.0429 (12)0.0093 (9)0.0215 (10)0.0023 (9)
C120.0314 (11)0.0158 (8)0.0308 (11)0.0030 (8)0.0125 (9)0.0035 (8)
C130.0163 (8)0.0228 (9)0.0206 (9)0.0031 (7)0.0068 (7)0.0015 (7)
C140.0262 (11)0.0322 (11)0.0346 (12)0.0111 (9)0.0032 (9)0.0092 (9)
C150.0204 (10)0.0501 (14)0.0359 (12)0.0028 (9)0.0138 (9)0.0070 (10)
C160.0251 (10)0.0216 (9)0.0170 (9)0.0023 (7)0.0067 (7)0.0030 (7)
C170.0265 (10)0.0297 (10)0.0225 (10)0.0011 (8)0.0004 (8)0.0014 (8)
C180.0349 (11)0.0349 (11)0.0196 (9)0.0047 (9)0.0129 (9)0.0049 (8)
C190.0232 (10)0.0308 (11)0.0384 (12)0.0068 (9)0.0056 (9)0.0130 (9)
C200.0225 (10)0.0318 (11)0.0387 (12)0.0014 (8)0.0125 (9)0.0101 (9)
C210.0176 (9)0.0291 (10)0.0332 (11)0.0018 (8)0.0029 (8)0.0006 (9)
C220.0186 (9)0.0160 (8)0.0225 (9)0.0001 (7)0.0108 (7)0.0014 (7)
Geometric parameters (Å, º) top
Fe1—Cl12.3806 (5)C9—H9C0.9800
Fe1—P12.3280 (5)C10—H101.0000
Fe1—P22.3094 (5)C10—C111.524 (3)
Fe1—P32.2607 (5)C10—C121.524 (3)
Fe1—N11.9776 (14)C11—H11A0.9800
Fe1—C221.7214 (19)C11—H11B0.9800
P1—C51.8312 (18)C11—H11C0.9800
P1—C71.8558 (18)C12—H12A0.9800
P1—C101.8618 (18)C12—H12B0.9800
P2—C61.8452 (18)C12—H12C0.9800
P2—C131.8533 (18)C13—H131.0000
P2—C161.8597 (19)C13—C141.534 (3)
P3—C191.830 (2)C13—C151.528 (3)
P3—C201.820 (2)C14—H14A0.9800
P3—C211.828 (2)C14—H14B0.9800
O1—C221.154 (2)C14—H14C0.9800
N1—C11.369 (2)C15—H15A0.9800
N1—C21.370 (2)C15—H15B0.9800
C1—C41.381 (2)C15—H15C0.9800
C1—C51.494 (2)C16—H161.0000
C2—C31.385 (2)C16—C171.538 (3)
C2—C61.487 (2)C16—C181.535 (3)
C3—H30.9500C17—H17A0.9800
C3—C41.419 (3)C17—H17B0.9800
C4—H40.9500C17—H17C0.9800
C5—H5A0.9900C18—H18A0.9800
C5—H5B0.9900C18—H18B0.9800
C6—H6A0.9900C18—H18C0.9800
C6—H6B0.9900C19—H19A0.9800
C7—H71.0000C19—H19B0.9800
C7—C81.527 (3)C19—H19C0.9800
C7—C91.519 (3)C20—H20A0.9800
C8—H8A0.9800C20—H20B0.9800
C8—H8B0.9800C20—H20C0.9800
C8—H8C0.9800C21—H21A0.9800
C9—H9A0.9800C21—H21B0.9800
C9—H9B0.9800C21—H21C0.9800
P1—Fe1—Cl194.968 (19)H9A—C9—H9C109.5
P2—Fe1—Cl186.636 (19)H9B—C9—H9C109.5
P2—Fe1—P1155.63 (2)P1—C10—H10107.0
P3—Fe1—Cl183.741 (19)C11—C10—P1114.34 (13)
P3—Fe1—P1101.40 (2)C11—C10—H10107.0
P3—Fe1—P2102.95 (2)C12—C10—P1112.31 (13)
N1—Fe1—Cl190.11 (4)C12—C10—H10107.0
N1—Fe1—P177.20 (4)C12—C10—C11108.70 (16)
N1—Fe1—P278.48 (4)C10—C11—H11A109.5
N1—Fe1—P3173.57 (4)C10—C11—H11B109.5
C22—Fe1—Cl1175.86 (6)C10—C11—H11C109.5
C22—Fe1—P187.76 (6)H11A—C11—H11B109.5
C22—Fe1—P292.16 (6)H11A—C11—H11C109.5
C22—Fe1—P392.68 (6)H11B—C11—H11C109.5
C22—Fe1—N193.54 (7)C10—C12—H12A109.5
C5—P1—Fe199.97 (6)C10—C12—H12B109.5
C5—P1—C7102.90 (9)C10—C12—H12C109.5
C5—P1—C10105.84 (8)H12A—C12—H12B109.5
C7—P1—Fe1113.43 (6)H12A—C12—H12C109.5
C7—P1—C10106.99 (8)H12B—C12—H12C109.5
C10—P1—Fe1124.92 (6)P2—C13—H13107.1
C6—P2—Fe1100.07 (6)C14—C13—P2114.00 (14)
C6—P2—C13102.29 (8)C14—C13—H13107.1
C6—P2—C16103.30 (9)C15—C13—P2112.97 (14)
C13—P2—Fe1122.86 (6)C15—C13—H13107.1
C13—P2—C16104.75 (8)C15—C13—C14108.20 (17)
C16—P2—Fe1120.00 (6)C13—C14—H14A109.5
C19—P3—Fe1117.86 (7)C13—C14—H14B109.5
C20—P3—Fe1116.29 (7)C13—C14—H14C109.5
C20—P3—C19100.34 (11)H14A—C14—H14B109.5
C20—P3—C21101.23 (10)H14A—C14—H14C109.5
C21—P3—Fe1119.75 (7)H14B—C14—H14C109.5
C21—P3—C1997.82 (10)C13—C15—H15A109.5
C1—N1—Fe1126.17 (12)C13—C15—H15B109.5
C1—N1—C2107.90 (14)C13—C15—H15C109.5
C2—N1—Fe1125.92 (12)H15A—C15—H15B109.5
N1—C1—C4109.38 (15)H15A—C15—H15C109.5
N1—C1—C5115.96 (15)H15B—C15—H15C109.5
C4—C1—C5134.66 (16)P2—C16—H16106.4
N1—C2—C3109.28 (16)C17—C16—P2112.55 (13)
N1—C2—C6116.10 (15)C17—C16—H16106.4
C3—C2—C6134.50 (16)C18—C16—P2115.61 (13)
C2—C3—H3126.7C18—C16—H16106.4
C2—C3—C4106.62 (16)C18—C16—C17108.91 (16)
C4—C3—H3126.7C16—C17—H17A109.5
C1—C4—C3106.81 (15)C16—C17—H17B109.5
C1—C4—H4126.6C16—C17—H17C109.5
C3—C4—H4126.6H17A—C17—H17B109.5
P1—C5—H5A111.1H17A—C17—H17C109.5
P1—C5—H5B111.1H17B—C17—H17C109.5
C1—C5—P1103.35 (12)C16—C18—H18A109.5
C1—C5—H5A111.1C16—C18—H18B109.5
C1—C5—H5B111.1C16—C18—H18C109.5
H5A—C5—H5B109.1H18A—C18—H18B109.5
P2—C6—H6A110.5H18A—C18—H18C109.5
P2—C6—H6B110.5H18B—C18—H18C109.5
C2—C6—P2106.13 (12)P3—C19—H19A109.5
C2—C6—H6A110.5P3—C19—H19B109.5
C2—C6—H6B110.5P3—C19—H19C109.5
H6A—C6—H6B108.7H19A—C19—H19B109.5
P1—C7—H7105.7H19A—C19—H19C109.5
C8—C7—P1116.35 (14)H19B—C19—H19C109.5
C8—C7—H7105.7P3—C20—H20A109.5
C9—C7—P1111.28 (14)P3—C20—H20B109.5
C9—C7—H7105.7P3—C20—H20C109.5
C9—C7—C8111.21 (18)H20A—C20—H20B109.5
C7—C8—H8A109.5H20A—C20—H20C109.5
C7—C8—H8B109.5H20B—C20—H20C109.5
C7—C8—H8C109.5P3—C21—H21A109.5
H8A—C8—H8B109.5P3—C21—H21B109.5
H8A—C8—H8C109.5P3—C21—H21C109.5
H8B—C8—H8C109.5H21A—C21—H21B109.5
C7—C9—H9A109.5H21A—C21—H21C109.5
C7—C9—H9B109.5H21B—C21—H21C109.5
C7—C9—H9C109.5O1—C22—Fe1179.33 (17)
H9A—C9—H9B109.5
Fe1—P1—C5—C140.89 (12)C4—C1—C5—P1149.24 (19)
Fe1—P1—C7—C8142.56 (14)C5—P1—C7—C835.53 (17)
Fe1—P1—C7—C988.66 (14)C5—P1—C7—C9164.30 (14)
Fe1—P1—C10—C11157.20 (12)C5—P1—C10—C1142.51 (16)
Fe1—P1—C10—C1232.73 (16)C5—P1—C10—C1281.96 (15)
Fe1—P2—C6—C234.85 (13)C5—C1—C4—C3177.90 (19)
Fe1—P2—C13—C14150.08 (12)C6—P2—C13—C1439.36 (16)
Fe1—P2—C13—C1585.85 (15)C6—P2—C13—C15163.43 (15)
Fe1—P2—C16—C1759.10 (15)C6—P2—C16—C1751.02 (15)
Fe1—P2—C16—C1866.94 (16)C6—P2—C16—C18177.06 (14)
Fe1—N1—C1—C4177.89 (12)C6—C2—C3—C4175.79 (19)
Fe1—N1—C1—C52.9 (2)C7—P1—C5—C176.14 (13)
Fe1—N1—C2—C3178.30 (12)C7—P1—C10—C1166.71 (16)
Fe1—N1—C2—C65.0 (2)C7—P1—C10—C12168.82 (13)
N1—C1—C4—C31.1 (2)C10—P1—C5—C1171.74 (12)
N1—C1—C5—P131.79 (18)C10—P1—C7—C875.74 (17)
N1—C2—C3—C40.1 (2)C10—P1—C7—C953.03 (16)
N1—C2—C6—P223.20 (19)C13—P2—C6—C2161.91 (12)
C1—N1—C2—C30.8 (2)C13—P2—C16—C17157.79 (14)
C1—N1—C2—C6175.95 (15)C13—P2—C16—C1876.18 (16)
C2—N1—C1—C41.2 (2)C16—P2—C6—C289.47 (13)
C2—N1—C1—C5178.04 (15)C16—P2—C13—C1468.15 (16)
C2—C3—C4—C10.6 (2)C16—P2—C13—C1555.92 (16)
C3—C2—C6—P2152.46 (19)
(II) {2,5-Bis[(diisopropylphosphanyl)methyl]pyrrolido-κ3P,N,P'}chlorido(pyridine-κN)iron(II) top
Crystal data top
[Fe(C18H34NP2)Cl(C5H5N)]F(000) = 1056
Mr = 496.80Dx = 1.244 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 7.6074 (6) ÅCell parameters from 9997 reflections
b = 18.2229 (15) Åθ = 2.2–26.4°
c = 19.1442 (16) ŵ = 0.80 mm1
β = 92.3658 (13)°T = 296 K
V = 2651.7 (4) Å3Block, yellow
Z = 40.60 × 0.36 × 0.36 mm
Data collection top
Bruker APEX-II CCD
diffractometer
5423 independent reflections
Radiation source: fine-focus sealed-tube5174 reflections with I > 2σ(I)
Detector resolution: 8.33 pixels mm-1Rint = 0.023
φ and ω scansθmax = 26.4°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
h = 99
Tmin = 0.639, Tmax = 0.745k = 2222
44868 measured reflectionsl = 2323
Refinement top
Refinement on F2Primary atom site location: iterative
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.021Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.054H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.025P)2 + 1.182P]
where P = (Fo2 + 2Fc2)/3
5423 reflections(Δ/σ)max = 0.001
270 parametersΔρmax = 0.28 e Å3
0 restraintsΔρmin = 0.23 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.42549 (2)0.28801 (2)0.43529 (2)0.01567 (5)
Cl10.15367 (4)0.33264 (2)0.46273 (2)0.02582 (7)
P10.33422 (4)0.15339 (2)0.45019 (2)0.02159 (7)
P20.52956 (4)0.40115 (2)0.36887 (2)0.01918 (7)
N10.57357 (13)0.23834 (6)0.36254 (5)0.0212 (2)
N20.57605 (12)0.29532 (5)0.53036 (5)0.01751 (19)
C10.55480 (16)0.16632 (7)0.34046 (7)0.0246 (3)
C20.65300 (15)0.27547 (7)0.30945 (6)0.0232 (2)
C30.67976 (16)0.22858 (8)0.25453 (7)0.0301 (3)
H30.72920.24050.21240.036*
C40.61773 (16)0.15886 (8)0.27451 (7)0.0310 (3)
H40.61920.11610.24810.037*
C50.48060 (18)0.10983 (7)0.38790 (7)0.0303 (3)
H5A0.57580.08490.41340.036*
H5B0.41510.07360.36030.036*
C60.70037 (16)0.35472 (7)0.31915 (6)0.0260 (3)
H6A0.70970.37810.27390.031*
H6B0.81340.35880.34420.031*
C70.3528 (3)0.09513 (7)0.52955 (7)0.0434 (4)
H70.33180.04400.51580.052*
C80.5372 (3)0.10094 (9)0.56399 (10)0.0642 (6)
H8A0.62310.08930.53040.096*
H8B0.54780.06720.60240.096*
H8C0.55630.15000.58080.096*
C90.2137 (3)0.11766 (10)0.58046 (8)0.0611 (6)
H9A0.22860.16850.59240.092*
H9B0.22610.08840.62210.092*
H9C0.09870.11030.55900.092*
C100.11042 (17)0.13506 (7)0.41300 (7)0.0281 (3)
H100.02750.15960.44310.034*
C110.0562 (2)0.05443 (9)0.40821 (8)0.0437 (4)
H11A0.13380.02870.37840.065*
H11B0.06230.05100.38920.065*
H11C0.06300.03290.45400.065*
C120.0912 (2)0.17101 (9)0.34094 (8)0.0380 (3)
H12A0.12330.22190.34460.057*
H12B0.02860.16700.32360.057*
H12C0.16690.14670.30940.057*
C130.63846 (15)0.48419 (7)0.40586 (7)0.0239 (2)
H130.54580.51530.42400.029*
C140.76244 (17)0.46424 (7)0.46777 (7)0.0302 (3)
H14A0.69860.43760.50180.045*
H14B0.81000.50830.48860.045*
H14C0.85660.43430.45180.045*
C150.73362 (19)0.52982 (8)0.35199 (8)0.0357 (3)
H15A0.82140.50020.33100.054*
H15B0.78890.57130.37470.054*
H15C0.65030.54660.31650.054*
C160.37789 (17)0.43727 (8)0.29881 (7)0.0295 (3)
H160.44770.46480.26580.035*
C170.2876 (2)0.37410 (10)0.25928 (9)0.0470 (4)
H17A0.37500.34230.24080.070*
H17B0.21430.39330.22160.070*
H17C0.21670.34690.29060.070*
C180.24214 (19)0.48941 (8)0.32810 (8)0.0383 (3)
H18A0.17650.46420.36250.057*
H18B0.16340.50590.29090.057*
H18C0.30110.53090.34930.057*
C190.75073 (16)0.28459 (7)0.53339 (7)0.0242 (2)
H190.80760.27690.49190.029*
C200.84954 (17)0.28449 (8)0.59556 (7)0.0299 (3)
H200.97050.27710.59570.036*
C210.76672 (18)0.29547 (8)0.65766 (7)0.0307 (3)
H210.83030.29520.70020.037*
C220.58713 (17)0.30679 (8)0.65485 (6)0.0290 (3)
H220.52760.31450.69570.035*
C230.49691 (15)0.30662 (7)0.59080 (6)0.0220 (2)
H230.37610.31470.58950.026*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01572 (8)0.01647 (9)0.01488 (8)0.00190 (6)0.00138 (6)0.00042 (6)
Cl10.01695 (13)0.02615 (15)0.03487 (16)0.00341 (11)0.00717 (11)0.00372 (12)
P10.02903 (16)0.01517 (14)0.02005 (15)0.00129 (11)0.00541 (12)0.00120 (11)
P20.01712 (14)0.02107 (15)0.01962 (14)0.00171 (11)0.00411 (11)0.00427 (11)
N10.0211 (5)0.0226 (5)0.0198 (5)0.0035 (4)0.0003 (4)0.0039 (4)
N20.0178 (5)0.0163 (4)0.0183 (5)0.0014 (3)0.0004 (4)0.0007 (4)
C10.0195 (6)0.0247 (6)0.0291 (6)0.0060 (5)0.0050 (5)0.0098 (5)
C20.0181 (5)0.0325 (7)0.0192 (5)0.0066 (5)0.0021 (4)0.0011 (5)
C30.0216 (6)0.0485 (8)0.0202 (6)0.0101 (6)0.0012 (5)0.0079 (6)
C40.0221 (6)0.0404 (8)0.0301 (7)0.0102 (5)0.0050 (5)0.0185 (6)
C50.0311 (7)0.0196 (6)0.0398 (7)0.0038 (5)0.0037 (6)0.0080 (5)
C60.0234 (6)0.0322 (7)0.0232 (6)0.0029 (5)0.0095 (5)0.0035 (5)
C70.0867 (12)0.0153 (6)0.0264 (7)0.0076 (7)0.0193 (7)0.0042 (5)
C80.1120 (17)0.0235 (8)0.0525 (10)0.0075 (9)0.0532 (11)0.0014 (7)
C90.1220 (18)0.0393 (9)0.0222 (7)0.0290 (10)0.0061 (9)0.0026 (6)
C100.0265 (6)0.0301 (7)0.0275 (6)0.0088 (5)0.0003 (5)0.0006 (5)
C110.0524 (9)0.0391 (8)0.0391 (8)0.0245 (7)0.0028 (7)0.0012 (7)
C120.0328 (7)0.0438 (8)0.0360 (8)0.0075 (6)0.0149 (6)0.0094 (6)
C130.0200 (6)0.0202 (6)0.0320 (6)0.0010 (4)0.0072 (5)0.0030 (5)
C140.0271 (6)0.0255 (6)0.0378 (7)0.0023 (5)0.0012 (5)0.0031 (5)
C150.0321 (7)0.0285 (7)0.0477 (8)0.0041 (6)0.0139 (6)0.0089 (6)
C160.0279 (6)0.0346 (7)0.0260 (6)0.0032 (5)0.0002 (5)0.0116 (5)
C170.0499 (9)0.0492 (9)0.0399 (8)0.0082 (8)0.0212 (7)0.0003 (7)
C180.0299 (7)0.0384 (8)0.0462 (8)0.0101 (6)0.0041 (6)0.0106 (7)
C190.0193 (6)0.0292 (6)0.0243 (6)0.0010 (5)0.0030 (5)0.0018 (5)
C200.0184 (6)0.0389 (8)0.0321 (7)0.0001 (5)0.0033 (5)0.0050 (6)
C210.0305 (7)0.0373 (7)0.0234 (6)0.0057 (5)0.0081 (5)0.0025 (5)
C220.0295 (7)0.0391 (7)0.0185 (6)0.0047 (6)0.0016 (5)0.0036 (5)
C230.0189 (5)0.0254 (6)0.0217 (6)0.0018 (5)0.0017 (4)0.0024 (5)
Geometric parameters (Å, º) top
Fe1—Cl12.3028 (3)C10—C111.5280 (19)
Fe1—P12.5688 (4)C10—C121.5287 (18)
Fe1—P22.5646 (4)C11—H11A0.9600
Fe1—N12.0391 (10)C11—H11B0.9600
Fe1—N22.1143 (10)C11—H11C0.9600
P1—C51.8444 (14)C12—H12A0.9600
P1—C71.8540 (14)C12—H12B0.9600
P1—C101.8485 (13)C12—H12C0.9600
P2—C61.8473 (12)C13—H130.9800
P2—C131.8519 (13)C13—C141.5278 (18)
P2—C161.8535 (13)C13—C151.5297 (17)
N1—C11.3843 (16)C14—H14A0.9600
N1—C21.3808 (16)C14—H14B0.9600
N2—C191.3420 (15)C14—H14C0.9600
N2—C231.3420 (15)C15—H15A0.9600
C1—C41.3752 (18)C15—H15B0.9600
C1—C51.4986 (19)C15—H15C0.9600
C2—C31.3765 (17)C16—H160.9800
C2—C61.4981 (18)C16—C171.525 (2)
C3—H30.9300C16—C181.5269 (19)
C3—C41.413 (2)C17—H17A0.9600
C4—H40.9300C17—H17B0.9600
C5—H5A0.9700C17—H17C0.9600
C5—H5B0.9700C18—H18A0.9600
C6—H6A0.9700C18—H18B0.9600
C6—H6B0.9700C18—H18C0.9600
C7—H70.9800C19—H190.9300
C7—C81.529 (2)C19—C201.3813 (18)
C7—C91.524 (3)C20—H200.9300
C8—H8A0.9600C20—C211.3828 (19)
C8—H8B0.9600C21—H210.9300
C8—H8C0.9600C21—C221.3805 (19)
C9—H9A0.9600C22—H220.9300
C9—H9B0.9600C22—C231.3803 (17)
C9—H9C0.9600C23—H230.9300
C10—H100.9800
Cl1—Fe1—P193.588 (12)P1—C10—H10107.2
Cl1—Fe1—P297.336 (12)C11—C10—P1116.05 (11)
P2—Fe1—P1155.950 (12)C11—C10—H10107.2
N1—Fe1—Cl1147.06 (3)C11—C10—C12110.02 (12)
N1—Fe1—P179.13 (3)C12—C10—P1108.80 (9)
N1—Fe1—P280.08 (3)C12—C10—H10107.2
N1—Fe1—N2108.72 (4)C10—C11—H11A109.5
N2—Fe1—Cl1103.95 (3)C10—C11—H11B109.5
N2—Fe1—P195.96 (3)C10—C11—H11C109.5
N2—Fe1—P2102.06 (3)H11A—C11—H11B109.5
C5—P1—Fe199.56 (4)H11A—C11—H11C109.5
C5—P1—C7104.82 (7)H11B—C11—H11C109.5
C5—P1—C10104.14 (6)C10—C12—H12A109.5
C7—P1—Fe1128.76 (4)C10—C12—H12B109.5
C10—P1—Fe1112.25 (4)C10—C12—H12C109.5
C10—P1—C7104.48 (7)H12A—C12—H12B109.5
C6—P2—Fe197.21 (4)H12A—C12—H12C109.5
C6—P2—C13104.96 (6)H12B—C12—H12C109.5
C6—P2—C16102.70 (6)P2—C13—H13107.0
C13—P2—Fe1127.57 (4)C14—C13—P2110.75 (8)
C13—P2—C16103.99 (6)C14—C13—H13107.0
C16—P2—Fe1116.65 (4)C14—C13—C15110.98 (11)
C1—N1—Fe1125.21 (8)C15—C13—P2113.77 (9)
C2—N1—Fe1123.78 (8)C15—C13—H13107.0
C2—N1—C1106.41 (10)C13—C14—H14A109.5
C19—N2—Fe1121.89 (8)C13—C14—H14B109.5
C19—N2—C23117.64 (10)C13—C14—H14C109.5
C23—N2—Fe1120.36 (8)H14A—C14—H14B109.5
N1—C1—C5120.19 (11)H14A—C14—H14C109.5
C4—C1—N1109.79 (12)H14B—C14—H14C109.5
C4—C1—C5129.99 (12)C13—C15—H15A109.5
N1—C2—C6119.44 (10)C13—C15—H15B109.5
C3—C2—N1109.94 (12)C13—C15—H15C109.5
C3—C2—C6130.59 (12)H15A—C15—H15B109.5
C2—C3—H3126.6H15A—C15—H15C109.5
C2—C3—C4106.84 (11)H15B—C15—H15C109.5
C4—C3—H3126.6P2—C16—H16108.1
C1—C4—C3107.00 (11)C17—C16—P2110.19 (10)
C1—C4—H4126.5C17—C16—H16108.1
C3—C4—H4126.5C17—C16—C18110.75 (12)
P1—C5—H5A109.6C18—C16—P2111.44 (10)
P1—C5—H5B109.6C18—C16—H16108.1
C1—C5—P1110.42 (8)C16—C17—H17A109.5
C1—C5—H5A109.6C16—C17—H17B109.5
C1—C5—H5B109.6C16—C17—H17C109.5
H5A—C5—H5B108.1H17A—C17—H17B109.5
P2—C6—H6A109.8H17A—C17—H17C109.5
P2—C6—H6B109.8H17B—C17—H17C109.5
C2—C6—P2109.55 (8)C16—C18—H18A109.5
C2—C6—H6A109.8C16—C18—H18B109.5
C2—C6—H6B109.8C16—C18—H18C109.5
H6A—C6—H6B108.2H18A—C18—H18B109.5
P1—C7—H7108.6H18A—C18—H18C109.5
C8—C7—P1110.56 (12)H18B—C18—H18C109.5
C8—C7—H7108.6N2—C19—H19118.7
C9—C7—P1109.77 (11)N2—C19—C20122.68 (11)
C9—C7—H7108.6C20—C19—H19118.7
C9—C7—C8110.76 (14)C19—C20—H20120.3
C7—C8—H8A109.5C19—C20—C21119.31 (12)
C7—C8—H8B109.5C21—C20—H20120.3
C7—C8—H8C109.5C20—C21—H21120.9
H8A—C8—H8B109.5C22—C21—C20118.26 (12)
H8A—C8—H8C109.5C22—C21—H21120.9
H8B—C8—H8C109.5C21—C22—H22120.4
C7—C9—H9A109.5C23—C22—C21119.30 (12)
C7—C9—H9B109.5C23—C22—H22120.4
C7—C9—H9C109.5N2—C23—C22122.81 (11)
H9A—C9—H9B109.5N2—C23—H23118.6
H9A—C9—H9C109.5C22—C23—H23118.6
H9B—C9—H9C109.5
Fe1—P1—C5—C115.25 (9)C5—P1—C7—C867.33 (12)
Fe1—P1—C7—C848.31 (15)C5—P1—C7—C9170.18 (11)
Fe1—P1—C7—C974.18 (13)C5—P1—C10—C1163.33 (12)
Fe1—P1—C10—C11170.07 (9)C5—P1—C10—C1261.35 (11)
Fe1—P1—C10—C1245.39 (11)C5—C1—C4—C3177.30 (12)
Fe1—P2—C6—C227.00 (9)C6—P2—C13—C1475.54 (10)
Fe1—P2—C13—C1436.14 (10)C6—P2—C13—C1550.28 (10)
Fe1—P2—C13—C15161.96 (7)C6—P2—C16—C1766.49 (11)
Fe1—P2—C16—C1738.40 (12)C6—P2—C16—C18170.15 (10)
Fe1—P2—C16—C1884.96 (10)C6—C2—C3—C4176.81 (12)
Fe1—N1—C1—C4155.35 (8)C7—P1—C5—C1149.78 (9)
Fe1—N1—C1—C526.61 (15)C7—P1—C10—C1146.40 (12)
Fe1—N1—C2—C3155.50 (8)C7—P1—C10—C12171.08 (10)
Fe1—N1—C2—C626.26 (15)C10—P1—C5—C1100.75 (10)
Fe1—N2—C19—C20175.74 (10)C10—P1—C7—C8176.56 (11)
Fe1—N2—C23—C22175.39 (10)C10—P1—C7—C960.95 (12)
N1—C1—C4—C30.49 (14)C13—P2—C6—C2159.06 (9)
N1—C1—C5—P126.75 (14)C13—P2—C16—C17175.70 (10)
N1—C2—C3—C41.16 (14)C13—P2—C16—C1860.95 (11)
N1—C2—C6—P236.72 (14)C16—P2—C6—C292.47 (9)
N2—C19—C20—C210.3 (2)C16—P2—C13—C14176.93 (9)
C1—N1—C2—C31.45 (13)C16—P2—C13—C1557.25 (10)
C1—N1—C2—C6176.78 (10)C19—N2—C23—C220.72 (18)
C2—N1—C1—C41.19 (13)C19—C20—C21—C220.5 (2)
C2—N1—C1—C5176.85 (10)C20—C21—C22—C230.1 (2)
C2—C3—C4—C10.41 (14)C21—C22—C23—N20.5 (2)
C3—C2—C6—P2145.46 (12)C23—N2—C19—C200.30 (18)
C4—C1—C5—P1155.66 (11)
(III) {2,5-Bis[(diisopropylphosphanyl)methyl]pyrrolido-κ3P,N,P'}dicarbonylchloridoiron(II) top
Crystal data top
[Fe(C18H34NP2)Cl(CO)2]F(000) = 1000
Mr = 473.72Dx = 1.389 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 13.7917 (17) ÅCell parameters from 9904 reflections
b = 14.6349 (18) Åθ = 2.3–28.1°
c = 11.2225 (13) ŵ = 0.94 mm1
β = 90.729 (2)°T = 120 K
V = 2265.0 (5) Å3Block, orange
Z = 40.23 × 0.20 × 0.17 mm
Data collection top
Bruker APEXII CCD
diffractometer
5626 independent reflections
Radiation source: fine-focus sealed-tube5123 reflections with I > 2σ(I)
Detector resolution: 8.33 pixels mm-1Rint = 0.041
φ and ω scansθmax = 28.3°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Krause et al., 2015)
h = 1818
Tmin = 0.678, Tmax = 0.746k = 1919
44037 measured reflectionsl = 1414
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090H-atom parameters constrained
S = 1.31 w = 1/[σ2(Fo2) + 4.0807P]
where P = (Fo2 + 2Fc2)/3
5626 reflections(Δ/σ)max = 0.001
279 parametersΔρmax = 0.60 e Å3
0 restraintsΔρmin = 0.48 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Fe10.73290 (2)0.49021 (2)0.34183 (3)0.01150 (8)
Cl1A0.6184 (2)0.5939 (2)0.2657 (3)0.0220 (6)0.3333
Cl10.84319 (11)0.38085 (11)0.41377 (12)0.0209 (3)0.6667
P10.79901 (4)0.58295 (4)0.48640 (5)0.01294 (12)
P20.70826 (4)0.41814 (4)0.16232 (5)0.01386 (12)
O20.5846 (3)0.6156 (3)0.2662 (4)0.0321 (11)0.6667
O2A0.8652 (7)0.3494 (5)0.4333 (9)0.028 (2)0.3333
O10.58964 (19)0.3980 (2)0.4889 (2)0.0574 (8)
N10.83295 (14)0.55086 (13)0.24775 (17)0.0147 (4)
C70.74777 (19)0.69742 (16)0.5135 (2)0.0189 (5)
H70.78600.72510.58070.023*
C100.82660 (19)0.53324 (17)0.6343 (2)0.0181 (5)
H100.85470.47140.61900.022*
C50.91928 (17)0.60593 (18)0.4245 (2)0.0179 (5)
H5A0.94220.66730.44900.022*
H5B0.96670.56000.45340.022*
C160.77215 (18)0.31139 (17)0.1253 (2)0.0200 (5)
H160.75140.29490.04230.024*
C110.7372 (2)0.51773 (19)0.7113 (2)0.0260 (6)
H11A0.71580.57620.74450.039*
H11B0.75360.47560.77640.039*
H11C0.68490.49140.66230.039*
C40.96296 (19)0.63374 (19)0.1981 (2)0.0226 (5)
H41.01970.67040.20380.027*
C130.58283 (19)0.40506 (19)0.1043 (2)0.0237 (5)
H130.55520.46820.10090.028*
C30.9176 (2)0.60232 (19)0.0924 (2)0.0245 (6)
H30.93820.61360.01330.029*
C60.7599 (2)0.50214 (18)0.0593 (2)0.0235 (5)
H6A0.78700.47090.01100.028*
H6B0.70910.54530.03170.028*
C80.7601 (2)0.75983 (18)0.4055 (2)0.0264 (6)
H8A0.82890.76320.38500.040*
H8B0.73630.82120.42440.040*
H8C0.72310.73520.33770.040*
C120.9043 (2)0.5865 (2)0.7040 (2)0.0251 (6)
H12A0.96360.58990.65700.038*
H12B0.91830.55530.77960.038*
H12C0.88070.64840.72010.038*
C190.6449 (2)0.4343 (2)0.4308 (2)0.0276 (6)
C90.6418 (2)0.6957 (2)0.5517 (3)0.0302 (6)
H9A0.60080.67620.48450.045*
H9B0.62230.75710.57710.045*
H9C0.63440.65290.61810.045*
C150.5780 (2)0.3690 (2)0.0230 (3)0.0306 (6)
H15A0.62340.40320.07240.046*
H15B0.51200.37660.05490.046*
H15C0.59530.30410.02350.046*
C170.7435 (2)0.23123 (19)0.2043 (3)0.0325 (7)
H17A0.76220.24440.28710.049*
H17B0.77680.17580.17770.049*
H17C0.67330.22190.19890.049*
C180.8820 (2)0.3239 (2)0.1225 (3)0.0302 (6)
H18A0.89780.37650.07220.045*
H18B0.91210.26880.09000.045*
H18C0.90670.33460.20360.045*
C140.5165 (2)0.3511 (3)0.1851 (3)0.0527 (11)
H14A0.53870.28750.18930.079*
H14B0.45010.35290.15290.079*
H14C0.51790.37790.26510.079*
C200.6421 (4)0.5689 (4)0.2971 (5)0.0198 (11)0.6667
C20A0.8107 (8)0.4104 (8)0.3908 (9)0.0185 (19)0.3333
C10.90896 (17)0.60093 (17)0.2917 (2)0.0158 (5)
C20.83779 (19)0.55196 (17)0.1258 (2)0.0184 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01164 (15)0.01116 (15)0.01167 (15)0.00031 (12)0.00145 (11)0.00019 (12)
Cl1A0.0203 (17)0.0172 (17)0.0281 (15)0.0109 (11)0.0154 (13)0.0062 (11)
Cl10.0247 (9)0.0195 (9)0.0183 (7)0.0029 (6)0.0020 (6)0.0022 (6)
P10.0128 (3)0.0138 (3)0.0122 (3)0.0000 (2)0.0003 (2)0.0021 (2)
P20.0144 (3)0.0141 (3)0.0131 (3)0.0017 (2)0.0021 (2)0.0014 (2)
O20.034 (3)0.028 (3)0.034 (2)0.0077 (18)0.016 (2)0.0050 (18)
O2A0.036 (5)0.015 (4)0.033 (4)0.010 (3)0.009 (3)0.004 (3)
O10.0497 (15)0.094 (2)0.0290 (12)0.0478 (15)0.0139 (11)0.0091 (13)
N10.0172 (10)0.0153 (9)0.0116 (9)0.0038 (8)0.0001 (7)0.0007 (7)
C70.0242 (13)0.0143 (11)0.0182 (12)0.0025 (9)0.0014 (10)0.0031 (9)
C100.0251 (13)0.0157 (11)0.0134 (11)0.0021 (9)0.0031 (9)0.0013 (9)
C50.0112 (10)0.0250 (12)0.0175 (12)0.0013 (9)0.0001 (9)0.0038 (10)
C160.0205 (12)0.0207 (12)0.0186 (12)0.0024 (10)0.0023 (10)0.0077 (10)
C110.0361 (15)0.0266 (13)0.0155 (12)0.0062 (12)0.0018 (11)0.0027 (10)
C40.0191 (12)0.0263 (13)0.0225 (13)0.0056 (10)0.0016 (10)0.0009 (10)
C130.0185 (12)0.0273 (14)0.0250 (13)0.0010 (10)0.0083 (10)0.0074 (11)
C30.0276 (14)0.0294 (14)0.0165 (12)0.0073 (11)0.0042 (10)0.0032 (10)
C60.0328 (14)0.0236 (13)0.0139 (11)0.0100 (11)0.0063 (10)0.0040 (10)
C80.0357 (15)0.0166 (12)0.0267 (14)0.0010 (11)0.0050 (12)0.0031 (10)
C120.0243 (13)0.0340 (15)0.0169 (12)0.0019 (11)0.0051 (10)0.0066 (11)
C190.0245 (14)0.0382 (16)0.0202 (13)0.0108 (12)0.0002 (11)0.0068 (12)
C90.0297 (15)0.0313 (15)0.0297 (15)0.0131 (12)0.0076 (12)0.0008 (12)
C150.0272 (14)0.0398 (17)0.0245 (14)0.0078 (13)0.0104 (11)0.0029 (12)
C170.0426 (18)0.0163 (13)0.0383 (17)0.0015 (12)0.0046 (14)0.0036 (12)
C180.0208 (13)0.0374 (16)0.0323 (16)0.0063 (12)0.0020 (11)0.0107 (13)
C140.0236 (16)0.105 (3)0.0301 (17)0.0275 (19)0.0019 (13)0.0096 (19)
C200.021 (3)0.022 (3)0.016 (3)0.007 (2)0.001 (2)0.0051 (19)
C20A0.019 (5)0.019 (5)0.017 (5)0.001 (4)0.001 (4)0.002 (4)
C10.0130 (11)0.0193 (11)0.0150 (11)0.0032 (9)0.0015 (9)0.0016 (9)
C20.0246 (13)0.0186 (11)0.0119 (11)0.0050 (10)0.0017 (9)0.0014 (9)
Geometric parameters (Å, º) top
Fe1—Cl1A2.343 (3)C11—H11C0.9800
Fe1—Cl12.3444 (19)C4—H40.9500
Fe1—P12.2953 (7)C4—C31.410 (4)
Fe1—P22.2954 (7)C4—C11.382 (3)
Fe1—N11.960 (2)C13—H131.0000
Fe1—C191.781 (3)C13—C151.523 (4)
Fe1—C201.770 (6)C13—C141.518 (4)
Fe1—C20A1.674 (12)C3—H30.9500
P1—C71.845 (2)C3—C21.381 (4)
P1—C101.847 (2)C6—H6A0.9900
P1—C51.838 (2)C6—H6B0.9900
P2—C161.844 (3)C6—C21.491 (3)
P2—C131.850 (3)C8—H8A0.9800
P2—C61.837 (3)C8—H8B0.9800
O2—C201.100 (6)C8—H8C0.9800
O2A—C20A1.258 (11)C12—H12A0.9800
O1—C191.140 (3)C12—H12B0.9800
N1—C11.366 (3)C12—H12C0.9800
N1—C21.372 (3)C9—H9A0.9800
C7—H71.0000C9—H9B0.9800
C7—C81.530 (4)C9—H9C0.9800
C7—C91.528 (4)C15—H15A0.9800
C10—H101.0000C15—H15B0.9800
C10—C111.532 (4)C15—H15C0.9800
C10—C121.533 (3)C17—H17A0.9800
C5—H5A0.9900C17—H17B0.9800
C5—H5B0.9900C17—H17C0.9800
C5—C11.497 (3)C18—H18A0.9800
C16—H161.0000C18—H18B0.9800
C16—C171.526 (4)C18—H18C0.9800
C16—C181.527 (4)C14—H14A0.9800
C11—H11A0.9800C14—H14B0.9800
C11—H11B0.9800C14—H14C0.9800
P1—Fe1—Cl1A97.74 (8)C3—C4—H4126.6
P1—Fe1—Cl184.84 (4)C1—C4—H4126.6
P1—Fe1—P2160.93 (3)C1—C4—C3106.8 (2)
P2—Fe1—Cl1A83.45 (8)P2—C13—H13105.8
P2—Fe1—Cl194.40 (4)C15—C13—P2113.30 (19)
N1—Fe1—Cl1A89.19 (11)C15—C13—H13105.8
N1—Fe1—Cl192.09 (7)C14—C13—P2114.3 (2)
N1—Fe1—P180.62 (6)C14—C13—H13105.8
N1—Fe1—P280.37 (6)C14—C13—C15111.1 (2)
C19—Fe1—Cl1A92.38 (14)C4—C3—H3126.5
C19—Fe1—Cl186.38 (11)C2—C3—C4107.0 (2)
C19—Fe1—P198.22 (9)C2—C3—H3126.5
C19—Fe1—P2100.75 (9)P2—C6—H6A110.3
C19—Fe1—N1178.17 (11)P2—C6—H6B110.3
C20—Fe1—Cl1174.79 (17)H6A—C6—H6B108.5
C20—Fe1—P195.12 (17)C2—C6—P2107.17 (17)
C20—Fe1—P287.34 (17)C2—C6—H6A110.3
C20—Fe1—N193.04 (18)C2—C6—H6B110.3
C20—Fe1—C1988.5 (2)C7—C8—H8A109.5
C20A—Fe1—Cl1A176.0 (4)C7—C8—H8B109.5
C20A—Fe1—P186.2 (3)C7—C8—H8C109.5
C20A—Fe1—P293.1 (3)H8A—C8—H8B109.5
C20A—Fe1—N192.3 (3)H8A—C8—H8C109.5
C20A—Fe1—C1986.2 (3)H8B—C8—H8C109.5
C7—P1—Fe1120.27 (8)C10—C12—H12A109.5
C7—P1—C10106.52 (11)C10—C12—H12B109.5
C10—P1—Fe1118.53 (8)C10—C12—H12C109.5
C5—P1—Fe1101.15 (8)H12A—C12—H12B109.5
C5—P1—C7104.22 (12)H12A—C12—H12C109.5
C5—P1—C10103.59 (12)H12B—C12—H12C109.5
C16—P2—Fe1121.43 (8)O1—C19—Fe1179.0 (3)
C16—P2—C13106.28 (12)C7—C9—H9A109.5
C13—P2—Fe1118.91 (9)C7—C9—H9B109.5
C6—P2—Fe1100.98 (8)C7—C9—H9C109.5
C6—P2—C16103.60 (13)H9A—C9—H9B109.5
C6—P2—C13102.47 (13)H9A—C9—H9C109.5
C1—N1—Fe1126.21 (16)H9B—C9—H9C109.5
C1—N1—C2107.9 (2)C13—C15—H15A109.5
C2—N1—Fe1125.90 (16)C13—C15—H15B109.5
P1—C7—H7107.0C13—C15—H15C109.5
C8—C7—P1111.37 (18)H15A—C15—H15B109.5
C8—C7—H7107.0H15A—C15—H15C109.5
C9—C7—P1113.66 (18)H15B—C15—H15C109.5
C9—C7—H7107.0C16—C17—H17A109.5
C9—C7—C8110.4 (2)C16—C17—H17B109.5
P1—C10—H10106.2C16—C17—H17C109.5
C11—C10—P1114.02 (18)H17A—C17—H17B109.5
C11—C10—H10106.2H17A—C17—H17C109.5
C11—C10—C12110.5 (2)H17B—C17—H17C109.5
C12—C10—P1113.15 (18)C16—C18—H18A109.5
C12—C10—H10106.2C16—C18—H18B109.5
P1—C5—H5A110.3C16—C18—H18C109.5
P1—C5—H5B110.3H18A—C18—H18B109.5
H5A—C5—H5B108.6H18A—C18—H18C109.5
C1—C5—P1107.01 (16)H18B—C18—H18C109.5
C1—C5—H5A110.3C13—C14—H14A109.5
C1—C5—H5B110.3C13—C14—H14B109.5
P2—C16—H16106.4C13—C14—H14C109.5
C17—C16—P2113.11 (19)H14A—C14—H14B109.5
C17—C16—H16106.4H14A—C14—H14C109.5
C17—C16—C18111.6 (2)H14B—C14—H14C109.5
C18—C16—P2112.32 (18)O2—C20—Fe1177.5 (6)
C18—C16—H16106.4O2A—C20A—Fe1176.0 (11)
C10—C11—H11A109.5N1—C1—C5116.6 (2)
C10—C11—H11B109.5N1—C1—C4109.3 (2)
C10—C11—H11C109.5C4—C1—C5134.0 (2)
H11A—C11—H11B109.5N1—C2—C3109.0 (2)
H11A—C11—H11C109.5N1—C2—C6116.7 (2)
H11B—C11—H11C109.5C3—C2—C6134.3 (2)
Fe1—P1—C7—C864.7 (2)C5—P1—C7—C847.6 (2)
Fe1—P1—C7—C960.8 (2)C5—P1—C7—C9173.05 (19)
Fe1—P1—C10—C1175.67 (19)C5—P1—C10—C11173.36 (18)
Fe1—P1—C10—C12156.94 (15)C5—P1—C10—C1246.0 (2)
Fe1—P1—C5—C128.94 (18)C16—P2—C13—C1547.1 (2)
Fe1—P2—C16—C1765.5 (2)C16—P2—C13—C1481.5 (3)
Fe1—P2—C16—C1861.9 (2)C16—P2—C6—C297.1 (2)
Fe1—P2—C13—C15171.46 (17)C4—C3—C2—N10.4 (3)
Fe1—P2—C13—C1459.9 (3)C4—C3—C2—C6179.0 (3)
Fe1—P2—C6—C229.3 (2)C13—P2—C16—C1774.7 (2)
Fe1—N1—C1—C53.2 (3)C13—P2—C16—C18157.84 (19)
Fe1—N1—C1—C4179.17 (17)C13—P2—C6—C2152.52 (19)
Fe1—N1—C2—C3179.30 (18)C3—C4—C1—N10.1 (3)
Fe1—N1—C2—C60.2 (3)C3—C4—C1—C5177.1 (3)
P1—C5—C1—N123.3 (3)C6—P2—C16—C17177.70 (19)
P1—C5—C1—C4159.9 (3)C6—P2—C16—C1850.3 (2)
P2—C6—C2—N121.7 (3)C6—P2—C13—C1561.3 (2)
P2—C6—C2—C3158.9 (3)C6—P2—C13—C14170.1 (2)
C7—P1—C10—C1163.8 (2)C1—N1—C2—C30.5 (3)
C7—P1—C10—C1263.6 (2)C1—N1—C2—C6179.0 (2)
C7—P1—C5—C196.51 (18)C1—C4—C3—C20.2 (3)
C10—P1—C7—C8156.73 (18)C2—N1—C1—C5178.0 (2)
C10—P1—C7—C977.8 (2)C2—N1—C1—C40.4 (3)
C10—P1—C5—C1152.21 (17)
 

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