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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2011 Feb 12;67(Pt 3):m331. doi: 10.1107/S160053681100465X

Dinitro­sylbis[tris­(4-methyl­phen­yl)phosphane]iron

Myron W Jones a,*, Douglas R Powell a, George B Richter-Addo a
PMCID: PMC3052133  PMID: 21522262

Abstract

The title compound, [Fe(NO)2(C21H21P)2], belongs to the family of metal dinitrosyl compounds with the general formula Fe(NO)2(L)x, referred to collectively as ‘dinitrosyl iron compounds’ (DNICs). Herein we report the structure of a dinitrosyl iron diphosphane complex, [Fe(NO)2 L 2], with L = P(C6H4-p-CH3)3. There are two crystallographically independent but chemically equal mol­ecules per asymmetric unit. The iron atom in each mol­ecule is tetra­hedrally coordinated by two phosphane ligands and two NO groups, with Fe—N—O angles in the range 173.84 (15)–179.31 (16)°.

Related literature

The starting compound, Fe(NO)2(CO)2, was prepared using a published method described by Eisch & King (1965 ▶). For the structures of some related dinitrosyl complexes, see: Li et al. (2003 ▶); Atkinson et al. (1996 ▶); Li Kam Wah et al. (1989 ▶); Albano et al. (1974 ▶). For general information on metal nitrosyl chemistry, see: Richter-Addo & Legzdins (1992 ▶).graphic file with name e-67-0m331-scheme1.jpg

Experimental

Crystal data

  • [Fe(NO)2(C21H21P)2]

  • M r = 724.57

  • Triclinic, Inline graphic

  • a = 10.240 (2) Å

  • b = 19.409 (4) Å

  • c = 21.040 (4) Å

  • α = 114.508 (5)°

  • β = 93.158 (6)°

  • γ = 94.732 (6)°

  • V = 3773.5 (13) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 0.52 mm−1

  • T = 100 K

  • 0.34 × 0.29 × 0.29 mm

Data collection

  • Bruker APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2001 ▶) T min = 0.843, T max = 0.863

  • 39881 measured reflections

  • 14767 independent reflections

  • 12772 reflections with I > 2σ(I)

  • R int = 0.025

Refinement

  • R[F 2 > 2σ(F 2)] = 0.035

  • wR(F 2) = 0.095

  • S = 1.01

  • 14767 reflections

  • 883 parameters

  • H-atom parameters constrained

  • Δρmax = 0.47 e Å−3

  • Δρmin = −0.26 e Å−3

Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681100465X/fk2034sup1.cif

e-67-0m331-sup1.cif (53KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S160053681100465X/fk2034Isup2.hkl

e-67-0m331-Isup2.hkl (721.8KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

We are grateful to the US Department of Education (GAANN Fellowship to MWJ; P200A030196) and the National Science Foundation (CHE-0076640 and CHE-0911537) for funding this work. The authors thank the National Science Foundation (CHE-0130835) and the University of Oklahoma for funds to acquire the diffractometer and computers used in this work.

supplementary crystallographic information

Comment

The molecular structure of the title compound is shown in Fig. 1. There are two distinct molecules per asymmetric unit of the cell. Each molecule possesses a distorted tetrahedral geometry around the iron center. The irons are bound to two nitrosyl groups via the nitrogen atoms and to two phosphine ligands via the phosphorous atoms. The Fe(NO)2 groups are in the attracto conformation where the bond angles O···Fe···O < N—Fe—N (Richter-Addo & Legzdins, 1992). The N—Fe—N bond angles for molecule 1 and molecule 2 are 129.89 (7)° and 124.29 (8)° respectively, while the interphosphine angles, P—Fe—P, are 106.00 (2)° and 105.57 (2)° respectively. The Fe—N—O bond angles range between 173.84 (15)° and 179.31 (16)°. For the structures of some related complexes, see: Li et al. (2003), Atkinson et al. (1996), Li Kam Wah et al. (1989), and Albano et al. (1974).

Experimental

Dark red Fe(NO)2(CO)2 (20 µL, 0.18 mmol) (Eisch & King, 1965) was added by syringe under nitrogen to a colorless toluene solution (5 ml) of P(C6H4-p-CH3)3 (0.111 g, 0.36 mmol) in a Schlenk tube. The mixture was stirred and heated to reflux under nitrogen for a period of ~3 h. A color change from light red to black/dark brown was observed within the first 30 min. The reaction was stopped when the infrared spectrum indicated the absence of characteristic carbonyl stretching frequencies for Fe(NO)2(CO)2 (νCO = 2090 cm-1 and 2040 cm-1). The reaction mixture was filtered through celite under N2 and the solvent was subsequently removed under vacuum. Isolated yield of the Fe(NO)2L2 compound: 31%. IR (toluene, cm-1): νNO = 1714 s and 1670 s. 31P{1H} NMR (CDCl3): δ 58.4 (s) referenced to 85% H3PO4. Suitable crystals for X-ray diffraction studies were grown by slow evaporation of a chloroform solution of the complex under nitrogen at ambient temperature.

Refinement

Phenyl H atoms were placed using known geometry with C—H = 0.95 Å. Methyl H atoms were initially located on a difference map and their positions were refined as rigid groups maintaining C—H = 0.98 Å and C—C—H angles to be equal by refining a torsion angle for each of the rigid groups. Once refinement had converged, the additional torsion angles were removed and refinement was repeated. Displacement parameters of phenyl H atoms were set to 1.2 times the isotropic equivalent for the bonded C (1.5 for methyl H atoms).

Figures

Fig. 1.

Fig. 1.

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The molecular structure of the title compound showing the relative orientation of the two neighboring molecules. Hydrogen atoms were omitted for clarity. The displacement ellipsoids were drawn at the 50% probability level.

Crystal data

[Fe(NO)2(C21H21P)2] Z = 4
Mr = 724.57 F(000) = 1520
Triclinic, P1 Dx = 1.275 Mg m−3
Hall symbol: -P 1 Mo Kα radiation, λ = 0.71073 Å
a = 10.240 (2) Å Cell parameters from 8062 reflections
b = 19.409 (4) Å θ = 2.3–28.3°
c = 21.040 (4) Å µ = 0.52 mm−1
α = 114.508 (5)° T = 100 K
β = 93.158 (6)° Prism, red
γ = 94.732 (6)° 0.34 × 0.29 × 0.29 mm
V = 3773.5 (13) Å3
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Data collection

Bruker APEX CCD diffractometer 14767 independent reflections
Radiation source: fine-focus sealed tube 12772 reflections with I > 2σ(I)
graphite Rint = 0.025
ω scans θmax = 26.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001) h = −12→12
Tmin = 0.843, Tmax = 0.863 k = −23→23
39881 measured reflections l = −25→25
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Refinement

Refinement on F2 Primary atom site location: structure-invariant direct methods
Least-squares matrix: full Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035 Hydrogen site location: geom and difmap
wR(F2) = 0.095 H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.052P)2 + 1.6P] where P = (Fo2 + 2Fc2)/3
14767 reflections (Δ/σ)max = 0.002
883 parameters Δρmax = 0.47 e Å−3
0 restraints Δρmin = −0.26 e Å−3
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Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

x y z Uiso*/Ueq
Fe1 0.39525 (2) 0.721825 (14) 0.379710 (13) 0.01684 (7)
P11 0.28352 (4) 0.75740 (2) 0.30476 (2) 0.01665 (10)
N11 0.52762 (15) 0.78538 (9) 0.40581 (8) 0.0229 (3)
O11 0.62231 (14) 0.83142 (9) 0.42413 (9) 0.0423 (4)
C101 0.38308 (17) 0.76140 (10) 0.23620 (9) 0.0187 (4)
C102 0.50084 (18) 0.72935 (11) 0.22635 (10) 0.0243 (4)
H102 0.5286 0.7048 0.2547 0.029*
C103 0.57844 (19) 0.73288 (12) 0.17537 (10) 0.0296 (4)
H103 0.6592 0.7112 0.1699 0.036*
C104 0.54089 (18) 0.76711 (11) 0.13254 (10) 0.0259 (4)
C105 0.42240 (19) 0.79844 (11) 0.14174 (10) 0.0272 (4)
H105 0.3939 0.8216 0.1124 0.033*
C106 0.34516 (18) 0.79640 (11) 0.19310 (10) 0.0239 (4)
H106 0.2654 0.8191 0.1991 0.029*
C107 0.6249 (2) 0.77143 (14) 0.07718 (11) 0.0379 (5)
H10A 0.6896 0.8169 0.0982 0.057*
H10B 0.5688 0.7744 0.0393 0.057*
H10C 0.6709 0.7258 0.0581 0.057*
C108 0.23570 (18) 0.85384 (10) 0.34316 (9) 0.0200 (4)
C109 0.3295 (2) 0.91604 (10) 0.35781 (10) 0.0251 (4)
H109 0.4153 0.9077 0.3434 0.030*
C110 0.2992 (2) 0.98989 (11) 0.39310 (11) 0.0340 (5)
H110 0.3646 1.0315 0.4027 0.041*
C111 0.1744 (2) 1.00388 (12) 0.41462 (11) 0.0393 (6)
C112 0.0815 (2) 0.94192 (13) 0.40057 (10) 0.0365 (5)
H112 −0.0040 0.9505 0.4154 0.044*
C113 0.11095 (19) 0.86772 (12) 0.36529 (10) 0.0269 (4)
H113 0.0457 0.8262 0.3562 0.032*
C114 0.1395 (3) 1.08414 (14) 0.45209 (15) 0.0675 (10)
H10D 0.0458 1.0851 0.4407 0.101*
H10E 0.1923 1.1181 0.4370 0.101*
H10F 0.1579 1.1013 0.5029 0.101*
C115 0.13121 (17) 0.69818 (10) 0.25660 (9) 0.0187 (4)
C116 0.04992 (18) 0.71691 (11) 0.21226 (10) 0.0260 (4)
H116 0.0735 0.7621 0.2063 0.031*
C117 −0.06413 (18) 0.67082 (11) 0.17700 (10) 0.0267 (4)
H117 −0.1170 0.6841 0.1462 0.032*
C118 −0.10355 (18) 0.60487 (11) 0.18570 (10) 0.0250 (4)
C119 −0.02243 (19) 0.58641 (10) 0.22993 (10) 0.0252 (4)
H119 −0.0468 0.5417 0.2366 0.030*
C120 0.09349 (18) 0.63199 (10) 0.26454 (9) 0.0214 (4)
H120 0.1479 0.6178 0.2941 0.026*
C121 −0.2297 (2) 0.55519 (12) 0.14826 (12) 0.0361 (5)
H10G −0.3037 0.5762 0.1748 0.054*
H10H −0.2242 0.5035 0.1445 0.054*
H10I −0.2432 0.5536 0.1012 0.054*
P12 0.27399 (4) 0.74526 (2) 0.47036 (2) 0.01681 (10)
N12 0.38322 (14) 0.62764 (9) 0.34965 (8) 0.0214 (3)
O12 0.37303 (14) 0.56049 (7) 0.33303 (8) 0.0337 (3)
C122 0.34119 (18) 0.70741 (10) 0.53047 (9) 0.0203 (4)
C123 0.47703 (19) 0.71779 (12) 0.54674 (10) 0.0280 (4)
H123 0.5321 0.7406 0.5242 0.034*
C124 0.5331 (2) 0.69512 (13) 0.59559 (11) 0.0352 (5)
H124 0.6258 0.7039 0.6069 0.042*
C125 0.4554 (2) 0.65974 (13) 0.62823 (11) 0.0323 (5)
C126 0.3199 (2) 0.64810 (11) 0.61068 (10) 0.0265 (4)
H126 0.2651 0.6231 0.6316 0.032*
C127 0.26342 (18) 0.67224 (10) 0.56331 (9) 0.0222 (4)
H127 0.1704 0.6647 0.5531 0.027*
C128 0.5146 (2) 0.63598 (17) 0.68217 (14) 0.0505 (7)
H10J 0.4522 0.6402 0.7169 0.076*
H10K 0.5962 0.6692 0.7057 0.076*
H10L 0.5340 0.5831 0.6590 0.076*
C129 0.10421 (17) 0.70029 (10) 0.44695 (9) 0.0185 (4)
C130 0.07860 (18) 0.62120 (10) 0.42010 (9) 0.0212 (4)
H130 0.1489 0.5918 0.4188 0.025*
C131 −0.04789 (18) 0.58485 (11) 0.39528 (10) 0.0242 (4)
H131 −0.0632 0.5309 0.3778 0.029*
C132 −0.15330 (18) 0.62621 (11) 0.39555 (10) 0.0260 (4)
C133 −0.12697 (18) 0.70518 (11) 0.42229 (10) 0.0262 (4)
H133 −0.1971 0.7346 0.4232 0.031*
C134 −0.00062 (18) 0.74192 (10) 0.44770 (9) 0.0218 (4)
H134 0.0145 0.7959 0.4658 0.026*
C135 −0.2907 (2) 0.58681 (12) 0.36654 (12) 0.0367 (5)
H10M −0.3544 0.6161 0.3968 0.055*
H10N −0.2975 0.5354 0.3649 0.055*
H10O −0.3094 0.5834 0.3191 0.055*
C136 0.26292 (17) 0.84432 (10) 0.53071 (9) 0.0185 (4)
C137 0.19553 (18) 0.86158 (11) 0.59036 (9) 0.0234 (4)
H137 0.1518 0.8215 0.5988 0.028*
C138 0.19201 (19) 0.93630 (11) 0.63711 (10) 0.0276 (4)
H138 0.1456 0.9469 0.6774 0.033*
C139 0.25514 (18) 0.99655 (11) 0.62653 (10) 0.0258 (4)
C140 0.32166 (19) 0.97939 (11) 0.56705 (10) 0.0246 (4)
H140 0.3648 1.0195 0.5585 0.029*
C141 0.32592 (18) 0.90400 (10) 0.51970 (9) 0.0214 (4)
H141 0.3725 0.8933 0.4794 0.026*
C142 0.2541 (2) 1.07824 (12) 0.67967 (11) 0.0372 (5)
H10P 0.1701 1.0837 0.7004 0.056*
H10Q 0.2652 1.1124 0.6563 0.056*
H10R 0.3265 1.0914 0.7167 0.056*
Fe2 0.20249 (2) 0.726480 (14) 0.861160 (13) 0.01703 (7)
P21 0.07337 (4) 0.78326 (2) 0.81153 (2) 0.01688 (10)
N21 0.19663 (14) 0.63819 (9) 0.80051 (8) 0.0217 (3)
O21 0.19345 (15) 0.57497 (8) 0.75630 (8) 0.0366 (4)
C201 −0.05695 (17) 0.83832 (10) 0.85539 (9) 0.0196 (4)
C202 −0.03062 (19) 0.88754 (10) 0.92638 (10) 0.0224 (4)
H202 0.0550 0.8936 0.9492 0.027*
C203 −0.1274 (2) 0.92766 (10) 0.96401 (10) 0.0267 (4)
H203 −0.1075 0.9607 1.0124 0.032*
C204 −0.25337 (19) 0.92016 (11) 0.93188 (11) 0.0294 (4)
C205 −0.27994 (19) 0.87105 (11) 0.86129 (11) 0.0296 (4)
H205 −0.3656 0.8651 0.8386 0.036*
C206 −0.18345 (18) 0.83046 (11) 0.82327 (10) 0.0245 (4)
H206 −0.2038 0.7971 0.7750 0.029*
C207 −0.3572 (2) 0.96526 (12) 0.97353 (13) 0.0422 (6)
H2OA −0.3894 0.9424 1.0042 0.063*
H20B −0.4305 0.9646 0.9413 0.063*
H20C −0.3189 1.0180 1.0021 0.063*
C208 −0.01124 (17) 0.71612 (10) 0.72718 (9) 0.0187 (4)
C209 −0.07366 (18) 0.64768 (10) 0.72364 (10) 0.0230 (4)
H209 −0.0690 0.6374 0.7641 0.028*
C210 −0.14236 (18) 0.59459 (11) 0.66173 (10) 0.0261 (4)
H210 −0.1848 0.5485 0.6604 0.031*
C211 −0.15029 (18) 0.60753 (11) 0.60152 (10) 0.0264 (4)
C212 −0.08842 (19) 0.67611 (11) 0.60524 (10) 0.0267 (4)
H212 −0.0929 0.6863 0.5648 0.032*
C213 −0.02019 (18) 0.72984 (11) 0.66754 (10) 0.0231 (4)
H213 0.0207 0.7764 0.6692 0.028*
C214 −0.2240 (2) 0.54858 (13) 0.53420 (11) 0.0407 (5)
H20D −0.2704 0.5742 0.5098 0.061*
H20E −0.2878 0.5155 0.5450 0.061*
H20F −0.1615 0.5178 0.5041 0.061*
C215 0.18434 (17) 0.84965 (10) 0.79286 (9) 0.0199 (4)
C216 0.1841 (2) 0.92808 (11) 0.82258 (10) 0.0267 (4)
H216 0.1147 0.9503 0.8495 0.032*
C217 0.2857 (2) 0.97461 (12) 0.81311 (11) 0.0341 (5)
H217 0.2855 1.0284 0.8347 0.041*
C218 0.3865 (2) 0.94394 (12) 0.77295 (11) 0.0329 (5)
C219 0.38517 (19) 0.86522 (12) 0.74230 (10) 0.0286 (4)
H219 0.4525 0.8430 0.7137 0.034*
C220 0.28759 (18) 0.81904 (11) 0.75285 (10) 0.0245 (4)
H220 0.2902 0.7654 0.7327 0.029*
C221 0.4951 (2) 0.99342 (15) 0.76049 (14) 0.0492 (6)
H20G 0.5807 0.9782 0.7694 0.074*
H20H 0.4915 1.0470 0.7923 0.074*
H20I 0.4834 0.9871 0.7118 0.074*
P22 0.09066 (4) 0.71480 (3) 0.94568 (2) 0.01739 (10)
N22 0.34007 (15) 0.78364 (9) 0.89869 (8) 0.0247 (3)
O22 0.44468 (15) 0.81869 (9) 0.92377 (10) 0.0486 (4)
C222 0.16869 (17) 0.65324 (10) 0.97918 (9) 0.0192 (4)
C223 0.30279 (17) 0.64885 (10) 0.97346 (9) 0.0207 (4)
H223 0.3474 0.6720 0.9476 0.025*
C224 0.37193 (18) 0.61113 (10) 1.00497 (10) 0.0227 (4)
H224 0.4634 0.6088 1.0004 0.027*
C225 0.31008 (19) 0.57673 (10) 1.04306 (10) 0.0244 (4)
C226 0.1750 (2) 0.57987 (12) 1.04768 (11) 0.0305 (5)
H226 0.1303 0.5558 1.0728 0.037*
C227 0.10521 (19) 0.61749 (11) 1.01627 (10) 0.0274 (4)
H227 0.0134 0.6190 1.0200 0.033*
C228 0.3873 (2) 0.53776 (12) 1.07865 (11) 0.0337 (5)
H20J 0.3826 0.5632 1.1295 0.051*
H20K 0.4794 0.5404 1.0686 0.051*
H20L 0.3501 0.4843 1.0611 0.051*
C229 0.08260 (17) 0.79809 (10) 1.02850 (9) 0.0197 (4)
C230 0.17595 (18) 0.86123 (10) 1.04769 (10) 0.0224 (4)
H230 0.2380 0.8623 1.0161 0.027*
C231 0.17944 (19) 0.92279 (11) 1.11262 (10) 0.0256 (4)
H231 0.2442 0.9654 1.1248 0.031*
C232 0.09016 (19) 0.92330 (11) 1.16006 (10) 0.0262 (4)
C233 −0.0038 (2) 0.86033 (12) 1.14066 (10) 0.0282 (4)
H233 −0.0663 0.8597 1.1722 0.034*
C234 −0.00769 (19) 0.79843 (11) 1.07609 (10) 0.0247 (4)
H234 −0.0723 0.7559 1.0641 0.030*
C235 0.0974 (2) 0.98930 (13) 1.23171 (11) 0.0366 (5)
H20M 0.0089 0.9947 1.2474 0.055*
H20N 0.1329 1.0363 1.2289 0.055*
H20O 0.1549 0.9796 1.2651 0.055*
C236 −0.07859 (17) 0.67165 (10) 0.91595 (9) 0.0189 (4)
C237 −0.10360 (18) 0.59358 (10) 0.87334 (10) 0.0221 (4)
H237 −0.0339 0.5626 0.8666 0.027*
C238 −0.22833 (18) 0.56068 (11) 0.84085 (10) 0.0231 (4)
H238 −0.2427 0.5075 0.8116 0.028*
C239 −0.33384 (17) 0.60460 (11) 0.85051 (9) 0.0217 (4)
C240 −0.30823 (18) 0.68238 (11) 0.89178 (10) 0.0227 (4)
H240 −0.3779 0.7134 0.8982 0.027*
C241 −0.18260 (17) 0.71601 (10) 0.92405 (9) 0.0211 (4)
H241 −0.1675 0.7695 0.9518 0.025*
C242 −0.47141 (18) 0.56809 (12) 0.81872 (10) 0.0277 (4)
H20P −0.5091 0.5424 0.8461 0.042*
H20Q −0.4685 0.5308 0.7702 0.042*
H20R −0.5261 0.6074 0.8192 0.042*
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Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23
Fe1 0.01472 (13) 0.01709 (13) 0.01718 (13) 0.00358 (10) 0.00093 (9) 0.00549 (10)
P11 0.0145 (2) 0.0170 (2) 0.0172 (2) 0.00310 (17) 0.00163 (17) 0.00579 (18)
N11 0.0184 (8) 0.0240 (8) 0.0253 (8) 0.0039 (6) −0.0006 (6) 0.0094 (7)
O11 0.0236 (8) 0.0363 (9) 0.0614 (11) −0.0091 (7) −0.0071 (7) 0.0188 (8)
C101 0.0159 (8) 0.0178 (9) 0.0177 (8) 0.0002 (7) 0.0020 (7) 0.0030 (7)
C102 0.0231 (10) 0.0258 (10) 0.0245 (10) 0.0072 (8) 0.0043 (8) 0.0100 (8)
C103 0.0206 (10) 0.0356 (11) 0.0297 (11) 0.0088 (8) 0.0081 (8) 0.0091 (9)
C104 0.0221 (10) 0.0282 (10) 0.0197 (9) −0.0035 (8) 0.0035 (7) 0.0036 (8)
C105 0.0248 (10) 0.0333 (11) 0.0235 (10) 0.0012 (8) 0.0026 (8) 0.0123 (8)
C106 0.0193 (9) 0.0298 (10) 0.0235 (9) 0.0059 (8) 0.0041 (7) 0.0113 (8)
C107 0.0297 (11) 0.0493 (14) 0.0320 (11) 0.0007 (10) 0.0116 (9) 0.0142 (10)
C108 0.0239 (9) 0.0213 (9) 0.0142 (8) 0.0079 (7) 0.0008 (7) 0.0060 (7)
C109 0.0281 (10) 0.0224 (10) 0.0231 (9) 0.0049 (8) −0.0005 (8) 0.0079 (8)
C110 0.0476 (13) 0.0210 (10) 0.0280 (11) 0.0041 (9) −0.0114 (9) 0.0067 (8)
C111 0.0509 (14) 0.0289 (11) 0.0260 (11) 0.0215 (10) −0.0137 (10) −0.0013 (9)
C112 0.0356 (12) 0.0434 (13) 0.0231 (10) 0.0248 (10) 0.0002 (9) 0.0033 (9)
C113 0.0255 (10) 0.0318 (11) 0.0218 (9) 0.0103 (8) 0.0018 (8) 0.0085 (8)
C114 0.076 (2) 0.0357 (14) 0.0576 (17) 0.0335 (14) −0.0298 (15) −0.0138 (12)
C115 0.0154 (8) 0.0198 (9) 0.0180 (8) 0.0030 (7) 0.0031 (7) 0.0048 (7)
C116 0.0215 (10) 0.0324 (11) 0.0285 (10) 0.0000 (8) −0.0004 (8) 0.0181 (9)
C117 0.0184 (9) 0.0369 (11) 0.0257 (10) 0.0035 (8) −0.0026 (8) 0.0147 (9)
C118 0.0186 (9) 0.0241 (10) 0.0232 (9) 0.0020 (7) 0.0001 (7) 0.0013 (8)
C119 0.0266 (10) 0.0172 (9) 0.0268 (10) 0.0011 (7) 0.0010 (8) 0.0049 (8)
C120 0.0214 (9) 0.0201 (9) 0.0200 (9) 0.0042 (7) −0.0003 (7) 0.0057 (7)
C121 0.0278 (11) 0.0294 (11) 0.0399 (12) −0.0030 (9) −0.0094 (9) 0.0062 (9)
P12 0.0159 (2) 0.0166 (2) 0.0169 (2) 0.00352 (17) 0.00099 (17) 0.00579 (18)
N12 0.0178 (8) 0.0222 (8) 0.0214 (8) 0.0061 (6) 0.0023 (6) 0.0056 (6)
O12 0.0325 (8) 0.0175 (7) 0.0456 (9) 0.0052 (6) 0.0036 (7) 0.0075 (6)
C122 0.0228 (9) 0.0187 (9) 0.0191 (9) 0.0061 (7) 0.0019 (7) 0.0068 (7)
C123 0.0219 (10) 0.0391 (12) 0.0298 (10) 0.0061 (8) 0.0038 (8) 0.0206 (9)
C124 0.0230 (10) 0.0535 (14) 0.0369 (12) 0.0113 (10) 0.0022 (9) 0.0257 (11)
C125 0.0337 (11) 0.0419 (12) 0.0284 (11) 0.0155 (9) 0.0040 (9) 0.0197 (10)
C126 0.0311 (11) 0.0267 (10) 0.0247 (10) 0.0067 (8) 0.0069 (8) 0.0128 (8)
C127 0.0222 (9) 0.0225 (9) 0.0205 (9) 0.0040 (7) 0.0021 (7) 0.0073 (8)
C128 0.0413 (14) 0.083 (2) 0.0514 (15) 0.0225 (13) 0.0079 (11) 0.0486 (15)
C129 0.0169 (9) 0.0206 (9) 0.0172 (8) 0.0032 (7) 0.0028 (7) 0.0068 (7)
C130 0.0191 (9) 0.0218 (9) 0.0229 (9) 0.0069 (7) 0.0026 (7) 0.0087 (8)
C131 0.0239 (10) 0.0200 (9) 0.0239 (9) 0.0014 (7) 0.0014 (8) 0.0046 (8)
C132 0.0192 (9) 0.0279 (10) 0.0244 (10) 0.0031 (8) 0.0003 (7) 0.0049 (8)
C133 0.0182 (9) 0.0287 (10) 0.0282 (10) 0.0089 (8) −0.0002 (8) 0.0076 (8)
C134 0.0232 (9) 0.0190 (9) 0.0207 (9) 0.0058 (7) 0.0016 (7) 0.0054 (7)
C135 0.0212 (10) 0.0334 (12) 0.0433 (13) 0.0006 (9) −0.0037 (9) 0.0054 (10)
C136 0.0164 (8) 0.0191 (9) 0.0173 (8) 0.0046 (7) −0.0013 (7) 0.0049 (7)
C137 0.0231 (10) 0.0237 (10) 0.0213 (9) 0.0024 (7) 0.0023 (7) 0.0075 (8)
C138 0.0255 (10) 0.0309 (11) 0.0194 (9) 0.0043 (8) 0.0042 (8) 0.0031 (8)
C139 0.0229 (10) 0.0233 (10) 0.0227 (9) 0.0048 (8) −0.0031 (8) 0.0017 (8)
C140 0.0258 (10) 0.0203 (9) 0.0246 (10) 0.0002 (7) −0.0030 (8) 0.0076 (8)
C141 0.0225 (9) 0.0219 (9) 0.0170 (9) 0.0035 (7) 0.0005 (7) 0.0054 (7)
C142 0.0373 (12) 0.0256 (11) 0.0342 (12) 0.0048 (9) 0.0022 (9) −0.0019 (9)
Fe2 0.01515 (13) 0.01775 (13) 0.01839 (13) 0.00327 (10) 0.00339 (10) 0.00735 (10)
P21 0.0166 (2) 0.0161 (2) 0.0176 (2) 0.00260 (17) 0.00314 (17) 0.00653 (18)
N21 0.0187 (8) 0.0225 (8) 0.0254 (8) 0.0051 (6) 0.0041 (6) 0.0108 (7)
O21 0.0392 (9) 0.0199 (7) 0.0389 (8) 0.0069 (6) 0.0010 (7) 0.0004 (6)
C201 0.0201 (9) 0.0175 (9) 0.0241 (9) 0.0033 (7) 0.0065 (7) 0.0107 (7)
C202 0.0248 (10) 0.0186 (9) 0.0242 (9) 0.0035 (7) 0.0036 (7) 0.0092 (8)
C203 0.0320 (11) 0.0187 (9) 0.0275 (10) 0.0030 (8) 0.0101 (8) 0.0071 (8)
C204 0.0262 (10) 0.0190 (9) 0.0419 (12) 0.0051 (8) 0.0146 (9) 0.0099 (9)
C205 0.0187 (10) 0.0265 (10) 0.0430 (12) 0.0047 (8) 0.0056 (8) 0.0132 (9)
C206 0.0221 (10) 0.0235 (10) 0.0270 (10) 0.0039 (8) 0.0035 (8) 0.0095 (8)
C207 0.0299 (12) 0.0288 (11) 0.0598 (15) 0.0077 (9) 0.0216 (11) 0.0079 (11)
C208 0.0154 (8) 0.0184 (9) 0.0197 (9) 0.0036 (7) 0.0029 (7) 0.0049 (7)
C209 0.0223 (9) 0.0224 (9) 0.0246 (9) 0.0044 (7) 0.0017 (7) 0.0099 (8)
C210 0.0232 (10) 0.0199 (9) 0.0322 (10) 0.0019 (7) 0.0008 (8) 0.0084 (8)
C211 0.0217 (10) 0.0269 (10) 0.0238 (10) 0.0029 (8) 0.0004 (8) 0.0043 (8)
C212 0.0255 (10) 0.0332 (11) 0.0206 (9) 0.0022 (8) 0.0025 (8) 0.0108 (8)
C213 0.0214 (9) 0.0231 (9) 0.0250 (9) 0.0004 (7) 0.0038 (7) 0.0104 (8)
C214 0.0450 (14) 0.0353 (12) 0.0289 (11) −0.0050 (10) −0.0072 (10) 0.0041 (10)
C215 0.0198 (9) 0.0215 (9) 0.0189 (9) −0.0006 (7) 0.0001 (7) 0.0097 (7)
C216 0.0342 (11) 0.0234 (10) 0.0218 (9) 0.0031 (8) 0.0036 (8) 0.0087 (8)
C217 0.0476 (13) 0.0205 (10) 0.0307 (11) −0.0071 (9) −0.0012 (10) 0.0098 (9)
C218 0.0303 (11) 0.0382 (12) 0.0308 (11) −0.0124 (9) −0.0062 (9) 0.0192 (10)
C219 0.0219 (10) 0.0405 (12) 0.0275 (10) 0.0012 (8) 0.0022 (8) 0.0190 (9)
C220 0.0244 (10) 0.0249 (10) 0.0253 (10) 0.0033 (8) 0.0035 (8) 0.0114 (8)
C221 0.0409 (14) 0.0538 (15) 0.0561 (16) −0.0189 (12) −0.0036 (12) 0.0317 (13)
P22 0.0158 (2) 0.0186 (2) 0.0188 (2) 0.00351 (17) 0.00334 (17) 0.00850 (18)
N22 0.0202 (8) 0.0242 (8) 0.0302 (9) 0.0030 (7) 0.0046 (7) 0.0117 (7)
O22 0.0238 (8) 0.0433 (10) 0.0653 (11) −0.0094 (7) 0.0005 (8) 0.0124 (9)
C222 0.0207 (9) 0.0175 (9) 0.0186 (9) 0.0038 (7) 0.0016 (7) 0.0065 (7)
C223 0.0204 (9) 0.0183 (9) 0.0228 (9) 0.0016 (7) 0.0025 (7) 0.0080 (7)
C224 0.0185 (9) 0.0212 (9) 0.0253 (9) 0.0026 (7) −0.0001 (7) 0.0070 (8)
C225 0.0285 (10) 0.0213 (9) 0.0232 (9) 0.0041 (8) −0.0006 (8) 0.0092 (8)
C226 0.0328 (11) 0.0348 (11) 0.0355 (11) 0.0083 (9) 0.0095 (9) 0.0248 (10)
C227 0.0217 (10) 0.0325 (11) 0.0344 (11) 0.0063 (8) 0.0073 (8) 0.0193 (9)
C228 0.0348 (12) 0.0356 (12) 0.0376 (12) 0.0076 (9) 0.0021 (9) 0.0218 (10)
C229 0.0197 (9) 0.0225 (9) 0.0190 (9) 0.0075 (7) 0.0021 (7) 0.0099 (7)
C230 0.0210 (9) 0.0253 (10) 0.0224 (9) 0.0051 (7) 0.0027 (7) 0.0109 (8)
C231 0.0241 (10) 0.0254 (10) 0.0245 (10) 0.0020 (8) −0.0040 (8) 0.0089 (8)
C232 0.0287 (10) 0.0299 (10) 0.0189 (9) 0.0123 (8) 0.0002 (8) 0.0078 (8)
C233 0.0292 (11) 0.0362 (11) 0.0226 (10) 0.0119 (9) 0.0083 (8) 0.0137 (9)
C234 0.0250 (10) 0.0273 (10) 0.0236 (9) 0.0054 (8) 0.0048 (8) 0.0118 (8)
C235 0.0402 (13) 0.0377 (12) 0.0244 (10) 0.0127 (10) 0.0035 (9) 0.0042 (9)
C236 0.0170 (9) 0.0235 (9) 0.0195 (9) 0.0028 (7) 0.0045 (7) 0.0118 (7)
C237 0.0183 (9) 0.0241 (9) 0.0263 (10) 0.0058 (7) 0.0054 (7) 0.0120 (8)
C238 0.0230 (9) 0.0218 (9) 0.0239 (9) 0.0003 (7) 0.0034 (7) 0.0092 (8)
C239 0.0185 (9) 0.0303 (10) 0.0198 (9) 0.0020 (7) 0.0024 (7) 0.0141 (8)
C240 0.0186 (9) 0.0300 (10) 0.0250 (9) 0.0073 (7) 0.0056 (7) 0.0160 (8)
C241 0.0217 (9) 0.0221 (9) 0.0217 (9) 0.0041 (7) 0.0060 (7) 0.0105 (8)
C242 0.0206 (10) 0.0366 (11) 0.0271 (10) 0.0009 (8) −0.0002 (8) 0.0154 (9)
Open in a new tab

Geometric parameters (Å, °)

Fe1—N11 1.6555 (16) Fe2—N21 1.6519 (16)
Fe1—N12 1.6590 (16) Fe2—N22 1.6529 (16)
Fe1—P12 2.2407 (6) Fe2—P22 2.2451 (6)
Fe1—P11 2.2600 (6) Fe2—P21 2.2574 (6)
P11—C108 1.8266 (18) P21—C208 1.8232 (18)
P11—C115 1.8288 (18) P21—C201 1.8242 (18)
P11—C101 1.8352 (18) P21—C215 1.8259 (18)
N11—O11 1.191 (2) N21—O21 1.190 (2)
C101—C102 1.389 (3) C201—C206 1.394 (3)
C101—C106 1.397 (3) C201—C202 1.395 (3)
C102—C103 1.390 (3) C202—C203 1.385 (3)
C102—H102 0.9500 C202—H202 0.9500
C103—C104 1.379 (3) C203—C204 1.390 (3)
C103—H103 0.9500 C203—H203 0.9500
C104—C105 1.389 (3) C204—C205 1.388 (3)
C104—C107 1.511 (3) C204—C207 1.511 (3)
C105—C106 1.385 (3) C205—C206 1.389 (3)
C105—H105 0.9500 C205—H205 0.9500
C106—H106 0.9500 C206—H206 0.9500
C107—H10A 0.9800 C207—H2OA 0.9799
C107—H10B 0.9798 C207—H20B 0.9800
C107—H10C 0.9801 C207—H20C 0.9800
C108—C113 1.393 (3) C208—C213 1.386 (3)
C108—C109 1.394 (3) C208—C209 1.397 (3)
C109—C110 1.385 (3) C209—C210 1.385 (3)
C109—H109 0.9500 C209—H209 0.9500
C110—C111 1.390 (3) C210—C211 1.390 (3)
C110—H110 0.9500 C210—H210 0.9500
C111—C112 1.387 (3) C211—C212 1.396 (3)
C111—C114 1.510 (3) C211—C214 1.510 (3)
C112—C113 1.388 (3) C212—C213 1.392 (3)
C112—H112 0.9500 C212—H212 0.9500
C113—H113 0.9500 C213—H213 0.9500
C114—H10D 0.9800 C214—H20D 0.9798
C114—H10E 0.9800 C214—H20E 0.9801
C114—H10F 0.9798 C214—H20F 0.9800
C115—C120 1.390 (3) C215—C216 1.385 (3)
C115—C116 1.393 (3) C215—C220 1.402 (3)
C116—C117 1.377 (3) C216—C217 1.398 (3)
C116—H116 0.9500 C216—H216 0.9500
C117—C118 1.397 (3) C217—C218 1.384 (3)
C117—H117 0.9500 C217—H217 0.9500
C118—C119 1.387 (3) C218—C219 1.389 (3)
C118—C121 1.507 (3) C218—C221 1.514 (3)
C119—C120 1.385 (3) C219—C220 1.376 (3)
C119—H119 0.9500 C219—H219 0.9500
C120—H120 0.9500 C220—H220 0.9500
C121—H10G 0.9800 C221—H20G 0.9801
C121—H10H 0.9799 C221—H20H 0.9800
C121—H10I 0.9800 C221—H20I 0.9802
P12—C129 1.8237 (18) P22—C236 1.8174 (18)
P12—C136 1.8298 (18) P22—C229 1.8323 (18)
P12—C122 1.8361 (18) P22—C222 1.8323 (18)
N12—O12 1.195 (2) N22—O22 1.187 (2)
C122—C123 1.392 (3) C222—C223 1.392 (3)
C122—C127 1.393 (3) C222—C227 1.394 (3)
C123—C124 1.390 (3) C223—C224 1.383 (3)
C123—H123 0.9500 C223—H223 0.9500
C124—C125 1.392 (3) C224—C225 1.385 (3)
C124—H124 0.9500 C224—H224 0.9500
C125—C126 1.391 (3) C225—C226 1.397 (3)
C125—C128 1.508 (3) C225—C228 1.504 (3)
C126—C127 1.384 (3) C226—C227 1.384 (3)
C126—H126 0.9500 C226—H226 0.9500
C127—H127 0.9500 C227—H227 0.9500
C128—H10J 0.9801 C228—H20J 0.9801
C128—H10K 0.9799 C228—H20K 0.9800
C128—H10L 0.9800 C228—H20L 0.9800
C129—C134 1.393 (2) C229—C230 1.390 (3)
C129—C130 1.394 (2) C229—C234 1.398 (3)
C130—C131 1.385 (3) C230—C231 1.389 (3)
C130—H130 0.9500 C230—H230 0.9500
C131—C132 1.396 (3) C231—C232 1.388 (3)
C131—H131 0.9500 C231—H231 0.9500
C132—C133 1.392 (3) C232—C233 1.391 (3)
C132—C135 1.509 (3) C232—C235 1.513 (3)
C133—C134 1.387 (3) C233—C234 1.386 (3)
C133—H133 0.9500 C233—H233 0.9500
C134—H134 0.9500 C234—H234 0.9500
C135—H10M 0.9800 C235—H20M 0.9800
C135—H10N 0.9800 C235—H20N 0.9800
C135—H10O 0.9798 C235—H20O 0.9799
C136—C141 1.388 (3) C236—C237 1.396 (3)
C136—C137 1.396 (3) C236—C241 1.398 (2)
C137—C138 1.379 (3) C237—C238 1.383 (3)
C137—H137 0.9500 C237—H237 0.9500
C138—C139 1.394 (3) C238—C239 1.403 (3)
C138—H138 0.9500 C238—H238 0.9500
C139—C140 1.388 (3) C239—C240 1.387 (3)
C139—C142 1.516 (3) C239—C242 1.507 (3)
C140—C141 1.393 (3) C240—C241 1.393 (3)
C140—H140 0.9500 C240—H240 0.9500
C141—H141 0.9500 C241—H241 0.9500
C142—H10P 0.9800 C242—H20P 0.9800
C142—H10Q 0.9800 C242—H20Q 0.9800
C142—H10R 0.9800 C242—H20R 0.9799
N11—Fe1—N12 129.89 (7) N21—Fe2—N22 124.29 (8)
N11—Fe1—P12 108.61 (6) N21—Fe2—P22 104.14 (6)
N12—Fe1—P12 98.23 (5) N22—Fe2—P22 108.24 (6)
N11—Fe1—P11 101.15 (6) N21—Fe2—P21 104.17 (6)
N12—Fe1—P11 111.19 (5) N22—Fe2—P21 108.98 (6)
P12—Fe1—P11 106.00 (2) P22—Fe2—P21 105.57 (2)
C108—P11—C115 103.82 (8) C208—P21—C201 102.89 (8)
C108—P11—C101 101.42 (8) C208—P21—C215 106.11 (8)
C115—P11—C101 104.38 (8) C201—P21—C215 105.07 (8)
C108—P11—Fe1 115.61 (6) C208—P21—Fe2 112.38 (6)
C115—P11—Fe1 117.49 (6) C201—P21—Fe2 123.08 (6)
C101—P11—Fe1 112.28 (6) C215—P21—Fe2 106.05 (6)
O11—N11—Fe1 179.31 (16) O21—N21—Fe2 179.10 (16)
C102—C101—C106 117.99 (16) C206—C201—C202 118.24 (17)
C102—C101—P11 119.80 (14) C206—C201—P21 123.77 (14)
C106—C101—P11 122.21 (13) C202—C201—P21 117.86 (14)
C101—C102—C103 120.56 (18) C203—C202—C201 120.95 (18)
C101—C102—H102 119.7 C203—C202—H202 119.5
C103—C102—H102 119.7 C201—C202—H202 119.5
C104—C103—C102 121.55 (18) C202—C203—C204 120.81 (18)
C104—C103—H103 119.2 C202—C203—H203 119.6
C102—C103—H103 119.2 C204—C203—H203 119.6
C103—C104—C105 118.00 (17) C205—C204—C203 118.35 (18)
C103—C104—C107 121.88 (19) C205—C204—C207 121.6 (2)
C105—C104—C107 120.12 (19) C203—C204—C207 120.06 (19)
C106—C105—C104 121.03 (18) C204—C205—C206 121.15 (19)
C106—C105—H105 119.5 C204—C205—H205 119.4
C104—C105—H105 119.5 C206—C205—H205 119.4
C105—C106—C101 120.86 (17) C205—C206—C201 120.49 (18)
C105—C106—H106 119.6 C205—C206—H206 119.8
C101—C106—H106 119.6 C201—C206—H206 119.8
C104—C107—H10A 109.5 C204—C207—H2OA 109.5
C104—C107—H10B 109.5 C204—C207—H20B 109.5
H10A—C107—H10B 109.5 H2OA—C207—H20B 109.5
C104—C107—H10C 109.5 C204—C207—H20C 109.5
H10A—C107—H10C 109.5 H2OA—C207—H20C 109.5
H10B—C107—H10C 109.5 H20B—C207—H20C 109.5
C113—C108—C109 118.39 (17) C213—C208—C209 118.54 (16)
C113—C108—P11 121.57 (15) C213—C208—P21 124.11 (14)
C109—C108—P11 119.68 (14) C209—C208—P21 117.32 (14)
C110—C109—C108 120.86 (19) C210—C209—C208 120.63 (18)
C110—C109—H109 119.6 C210—C209—H209 119.7
C108—C109—H109 119.6 C208—C209—H209 119.7
C109—C110—C111 120.8 (2) C209—C210—C211 121.13 (18)
C109—C110—H110 119.6 C209—C210—H210 119.4
C111—C110—H110 119.6 C211—C210—H210 119.4
C112—C111—C110 118.27 (19) C210—C211—C212 118.17 (17)
C112—C111—C114 120.4 (2) C210—C211—C214 120.45 (18)
C110—C111—C114 121.4 (2) C212—C211—C214 121.38 (18)
C111—C112—C113 121.3 (2) C213—C212—C211 120.82 (18)
C111—C112—H112 119.4 C213—C212—H212 119.6
C113—C112—H112 119.4 C211—C212—H212 119.6
C112—C113—C108 120.4 (2) C208—C213—C212 120.70 (17)
C112—C113—H113 119.8 C208—C213—H213 119.7
C108—C113—H113 119.8 C212—C213—H213 119.7
C111—C114—H10D 109.5 C211—C214—H20D 109.5
C111—C114—H10E 109.5 C211—C214—H20E 109.5
H10D—C114—H10E 109.5 H20D—C214—H20E 109.5
C111—C114—H10F 109.5 C211—C214—H20F 109.5
H10D—C114—H10F 109.5 H20D—C214—H20F 109.5
H10E—C114—H10F 109.5 H20E—C214—H20F 109.5
C120—C115—C116 118.13 (16) C216—C215—C220 118.19 (17)
C120—C115—P11 119.21 (13) C216—C215—P21 124.84 (14)
C116—C115—P11 122.66 (14) C220—C215—P21 116.40 (14)
C117—C116—C115 120.86 (18) C215—C216—C217 120.13 (19)
C117—C116—H116 119.6 C215—C216—H216 119.9
C115—C116—H116 119.6 C217—C216—H216 119.9
C116—C117—C118 121.21 (18) C218—C217—C216 121.34 (19)
C116—C117—H117 119.4 C218—C217—H217 119.3
C118—C117—H117 119.4 C216—C217—H217 119.3
C119—C118—C117 117.77 (17) C217—C218—C219 118.31 (18)
C119—C118—C121 120.96 (18) C217—C218—C221 122.0 (2)
C117—C118—C121 121.28 (18) C219—C218—C221 119.7 (2)
C120—C119—C118 121.14 (18) C220—C219—C218 120.81 (19)
C120—C119—H119 119.4 C220—C219—H219 119.6
C118—C119—H119 119.4 C218—C219—H219 119.6
C119—C120—C115 120.88 (17) C219—C220—C215 121.18 (18)
C119—C120—H120 119.6 C219—C220—H220 119.4
C115—C120—H120 119.6 C215—C220—H220 119.4
C118—C121—H10G 109.5 C218—C221—H20G 109.5
C118—C121—H10H 109.5 C218—C221—H20H 109.5
H10G—C121—H10H 109.5 H20G—C221—H20H 109.5
C118—C121—H10I 109.5 C218—C221—H20I 109.5
H10G—C121—H10I 109.5 H20G—C221—H20I 109.5
H10H—C121—H10I 109.5 H20H—C221—H20I 109.5
C129—P12—C136 105.07 (8) C236—P22—C229 105.45 (8)
C129—P12—C122 103.58 (8) C236—P22—C222 105.88 (8)
C136—P12—C122 101.37 (8) C229—P22—C222 99.71 (8)
C129—P12—Fe1 115.06 (6) C236—P22—Fe2 113.70 (6)
C136—P12—Fe1 118.82 (6) C229—P22—Fe2 120.17 (6)
C122—P12—Fe1 111.08 (6) C222—P22—Fe2 110.27 (6)
O12—N12—Fe1 175.05 (15) O22—N22—Fe2 173.84 (15)
C123—C122—C127 118.20 (17) C223—C222—C227 118.43 (17)
C123—C122—P12 118.11 (14) C223—C222—P22 117.38 (13)
C127—C122—P12 123.62 (14) C227—C222—P22 123.83 (14)
C124—C123—C122 120.77 (18) C224—C223—C222 120.75 (17)
C124—C123—H123 119.6 C224—C223—H223 119.6
C122—C123—H123 119.6 C222—C223—H223 119.6
C123—C124—C125 121.02 (19) C223—C224—C225 121.15 (17)
C123—C124—H124 119.5 C223—C224—H224 119.4
C125—C124—H124 119.5 C225—C224—H224 119.4
C126—C125—C124 117.95 (18) C224—C225—C226 118.11 (17)
C126—C125—C128 120.5 (2) C224—C225—C228 120.54 (18)
C124—C125—C128 121.6 (2) C226—C225—C228 121.34 (18)
C127—C126—C125 121.20 (18) C227—C226—C225 121.02 (18)
C127—C126—H126 119.4 C227—C226—H226 119.5
C125—C126—H126 119.4 C225—C226—H226 119.5
C126—C127—C122 120.83 (18) C226—C227—C222 120.50 (18)
C126—C127—H127 119.6 C226—C227—H227 119.7
C122—C127—H127 119.6 C222—C227—H227 119.7
C125—C128—H10J 109.5 C225—C228—H20J 109.5
C125—C128—H10K 109.5 C225—C228—H20K 109.5
H10J—C128—H10K 109.5 H20J—C228—H20K 109.5
C125—C128—H10L 109.5 C225—C228—H20L 109.5
H10J—C128—H10L 109.5 H20J—C228—H20L 109.5
H10K—C128—H10L 109.5 H20K—C228—H20L 109.5
C134—C129—C130 118.29 (16) C230—C229—C234 118.28 (17)
C134—C129—P12 121.71 (14) C230—C229—P22 119.14 (14)
C130—C129—P12 119.61 (13) C234—C229—P22 122.39 (14)
C131—C130—C129 120.95 (17) C231—C230—C229 120.67 (18)
C131—C130—H130 119.5 C231—C230—H230 119.7
C129—C130—H130 119.5 C229—C230—H230 119.7
C130—C131—C132 121.04 (17) C232—C231—C230 121.23 (18)
C130—C131—H131 119.5 C232—C231—H231 119.4
C132—C131—H131 119.5 C230—C231—H231 119.4
C133—C132—C131 117.70 (17) C231—C232—C233 118.07 (18)
C133—C132—C135 120.95 (17) C231—C232—C235 121.01 (19)
C131—C132—C135 121.34 (18) C233—C232—C235 120.89 (18)
C134—C133—C132 121.49 (17) C234—C233—C232 121.15 (18)
C134—C133—H133 119.3 C234—C233—H233 119.4
C132—C133—H133 119.3 C232—C233—H233 119.4
C133—C134—C129 120.52 (17) C233—C234—C229 120.60 (18)
C133—C134—H134 119.7 C233—C234—H234 119.7
C129—C134—H134 119.7 C229—C234—H234 119.7
C132—C135—H10M 109.5 C232—C235—H20M 109.5
C132—C135—H10N 109.5 C232—C235—H20N 109.5
H10M—C135—H10N 109.5 H20M—C235—H20N 109.5
C132—C135—H10O 109.5 C232—C235—H20O 109.5
H10M—C135—H10O 109.5 H20M—C235—H20O 109.5
H10N—C135—H10O 109.5 H20N—C235—H20O 109.5
C141—C136—C137 118.48 (16) C237—C236—C241 118.21 (16)
C141—C136—P12 120.68 (13) C237—C236—P22 119.27 (13)
C137—C136—P12 120.79 (14) C241—C236—P22 121.57 (14)
C138—C137—C136 120.50 (18) C238—C237—C236 121.00 (17)
C138—C137—H137 119.7 C238—C237—H237 119.5
C136—C137—H137 119.7 C236—C237—H237 119.5
C137—C138—C139 121.40 (18) C237—C238—C239 120.98 (17)
C137—C138—H138 119.3 C237—C238—H238 119.5
C139—C138—H138 119.3 C239—C238—H238 119.5
C140—C139—C138 118.09 (17) C240—C239—C238 117.90 (17)
C140—C139—C142 121.17 (19) C240—C239—C242 121.04 (17)
C138—C139—C142 120.72 (18) C238—C239—C242 121.04 (17)
C139—C140—C141 120.80 (18) C239—C240—C241 121.39 (17)
C139—C140—H140 119.6 C239—C240—H240 119.3
C141—C140—H140 119.6 C241—C240—H240 119.3
C136—C141—C140 120.72 (17) C240—C241—C236 120.48 (17)
C136—C141—H141 119.6 C240—C241—H241 119.8
C140—C141—H141 119.6 C236—C241—H241 119.8
C139—C142—H10P 109.5 C239—C242—H20P 109.5
C139—C142—H10Q 109.5 C239—C242—H20Q 109.5
H10P—C142—H10Q 109.5 H20P—C242—H20Q 109.5
C139—C142—H10R 109.5 C239—C242—H20R 109.5
H10P—C142—H10R 109.5 H20P—C242—H20R 109.5
H10Q—C142—H10R 109.5 H20Q—C242—H20R 109.5
N11—Fe1—P11—C108 −61.00 (9) N22—Fe2—P21—C208 140.90 (8)
N12—Fe1—P11—C108 157.97 (9) P22—Fe2—P21—C208 −103.03 (6)
P12—Fe1—P11—C108 52.26 (7) N21—Fe2—P21—C201 130.16 (9)
N11—Fe1—P11—C115 175.76 (8) N22—Fe2—P21—C201 −95.31 (9)
N12—Fe1—P11—C115 34.73 (9) P22—Fe2—P21—C201 20.77 (7)
P12—Fe1—P11—C115 −70.98 (7) N21—Fe2—P21—C215 −109.16 (8)
N11—Fe1—P11—C101 54.71 (8) N22—Fe2—P21—C215 25.38 (8)
N12—Fe1—P11—C101 −86.32 (8) P22—Fe2—P21—C215 141.45 (6)
P12—Fe1—P11—C101 167.97 (6) N22—Fe2—N21—O21 −53 (11)
N12—Fe1—N11—O11 130 (19) P22—Fe2—N21—O21 −178 (100)
P12—Fe1—N11—O11 −112 (19) P21—Fe2—N21—O21 72 (11)
C108—P11—C101—C102 136.85 (15) C208—P21—C201—C206 −5.77 (17)
C115—P11—C101—C102 −115.49 (15) C215—P21—C201—C206 105.11 (16)
Fe1—P11—C101—C102 12.83 (16) Fe2—P21—C201—C206 −133.75 (14)
C108—P11—C101—C106 −42.70 (16) C208—P21—C201—C202 170.03 (14)
C115—P11—C101—C106 64.96 (16) C215—P21—C201—C202 −79.08 (15)
Fe1—P11—C101—C106 −166.71 (13) Fe2—P21—C201—C202 42.06 (16)
C106—C101—C102—C103 0.5 (3) C206—C201—C202—C203 −0.1 (3)
P11—C101—C102—C103 −179.03 (15) P21—C201—C202—C203 −176.12 (14)
C101—C102—C103—C104 −0.9 (3) C201—C202—C203—C204 −0.3 (3)
C102—C103—C104—C105 0.1 (3) C202—C203—C204—C205 0.5 (3)
C102—C103—C104—C107 179.78 (18) C202—C203—C204—C207 −179.12 (18)
C103—C104—C105—C106 0.9 (3) C203—C204—C205—C206 −0.3 (3)
C107—C104—C105—C106 −178.73 (18) C207—C204—C205—C206 179.30 (19)
C104—C105—C106—C101 −1.3 (3) C204—C205—C206—C201 −0.1 (3)
C102—C101—C106—C105 0.5 (3) C202—C201—C206—C205 0.3 (3)
P11—C101—C106—C105 −179.94 (14) P21—C201—C206—C205 176.06 (15)
C115—P11—C108—C113 33.99 (17) C201—P21—C208—C213 90.85 (16)
C101—P11—C108—C113 142.08 (15) C215—P21—C208—C213 −19.25 (18)
Fe1—P11—C108—C113 −96.19 (15) Fe2—P21—C208—C213 −134.73 (14)
C115—P11—C108—C109 −152.98 (14) C201—P21—C208—C209 −87.29 (15)
C101—P11—C108—C109 −44.89 (16) C215—P21—C208—C209 162.61 (14)
Fe1—P11—C108—C109 76.84 (15) Fe2—P21—C208—C209 47.13 (15)
C113—C108—C109—C110 −0.4 (3) C213—C208—C209—C210 0.3 (3)
P11—C108—C109—C110 −173.66 (15) P21—C208—C209—C210 178.59 (14)
C108—C109—C110—C111 −0.2 (3) C208—C209—C210—C211 0.5 (3)
C109—C110—C111—C112 0.8 (3) C209—C210—C211—C212 −0.8 (3)
C109—C110—C111—C114 −179.0 (2) C209—C210—C211—C214 179.14 (19)
C110—C111—C112—C113 −0.7 (3) C210—C211—C212—C213 0.3 (3)
C114—C111—C112—C113 179.0 (2) C214—C211—C212—C213 −179.66 (19)
C111—C112—C113—C108 0.1 (3) C209—C208—C213—C212 −0.9 (3)
C109—C108—C113—C112 0.5 (3) P21—C208—C213—C212 −178.98 (14)
P11—C108—C113—C112 173.58 (15) C211—C212—C213—C208 0.6 (3)
C108—P11—C115—C120 −132.53 (14) C208—P21—C215—C216 123.32 (16)
C101—P11—C115—C120 121.59 (15) C201—P21—C215—C216 14.76 (18)
Fe1—P11—C115—C120 −3.49 (16) Fe2—P21—C215—C216 −116.98 (16)
C108—P11—C115—C116 46.96 (17) C208—P21—C215—C220 −65.58 (16)
C101—P11—C115—C116 −58.92 (17) C201—P21—C215—C220 −174.14 (14)
Fe1—P11—C115—C116 176.00 (13) Fe2—P21—C215—C220 54.13 (15)
C120—C115—C116—C117 −0.4 (3) C220—C215—C216—C217 −0.8 (3)
P11—C115—C116—C117 −179.90 (15) P21—C215—C216—C217 170.19 (15)
C115—C116—C117—C118 1.5 (3) C215—C216—C217—C218 1.5 (3)
C116—C117—C118—C119 −1.4 (3) C216—C217—C218—C219 −0.4 (3)
C116—C117—C118—C121 178.78 (19) C216—C217—C218—C221 178.2 (2)
C117—C118—C119—C120 0.3 (3) C217—C218—C219—C220 −1.3 (3)
C121—C118—C119—C120 −179.88 (18) C221—C218—C219—C220 179.96 (19)
C118—C119—C120—C115 0.8 (3) C218—C219—C220—C215 2.1 (3)
C116—C115—C120—C119 −0.7 (3) C216—C215—C220—C219 −1.0 (3)
P11—C115—C120—C119 178.82 (14) P21—C215—C220—C219 −172.70 (15)
N11—Fe1—P12—C129 163.18 (8) N21—Fe2—P22—C236 −59.05 (8)
N12—Fe1—P12—C129 −59.73 (8) N22—Fe2—P22—C236 166.94 (8)
P11—Fe1—P12—C129 55.19 (7) P21—Fe2—P22—C236 50.36 (7)
N11—Fe1—P12—C136 37.38 (9) N21—Fe2—P22—C229 174.68 (8)
N12—Fe1—P12—C136 174.47 (8) N22—Fe2—P22—C229 40.67 (9)
P11—Fe1—P12—C136 −70.61 (7) P21—Fe2—P22—C229 −75.91 (7)
N11—Fe1—P12—C122 −79.57 (9) N21—Fe2—P22—C222 59.68 (8)
N12—Fe1—P12—C122 57.52 (8) N22—Fe2—P22—C222 −74.34 (9)
P11—Fe1—P12—C122 172.44 (6) P21—Fe2—P22—C222 169.09 (6)
N11—Fe1—N12—O12 97.0 (16) N21—Fe2—N22—O22 −21.2 (15)
P12—Fe1—N12—O12 −25.7 (16) P22—Fe2—N22—O22 101.2 (15)
P11—Fe1—N12—O12 −136.5 (16) P21—Fe2—N22—O22 −144.4 (15)
C129—P12—C122—C123 166.66 (15) C236—P22—C222—C223 149.46 (14)
C136—P12—C122—C123 −84.59 (16) C229—P22—C222—C223 −101.29 (15)
Fe1—P12—C122—C123 42.60 (16) Fe2—P22—C222—C223 26.06 (15)
C129—P12—C122—C127 −16.60 (17) C236—P22—C222—C227 −37.58 (18)
C136—P12—C122—C127 92.15 (16) C229—P22—C222—C227 71.67 (17)
Fe1—P12—C122—C127 −140.65 (14) Fe2—P22—C222—C227 −160.98 (15)
C127—C122—C123—C124 −1.4 (3) C227—C222—C223—C224 −1.2 (3)
P12—C122—C123—C124 175.54 (16) P22—C222—C223—C224 172.13 (14)
C122—C123—C124—C125 1.6 (3) C222—C223—C224—C225 0.0 (3)
C123—C124—C125—C126 −0.3 (3) C223—C224—C225—C226 1.2 (3)
C123—C124—C125—C128 −179.0 (2) C223—C224—C225—C228 −178.34 (18)
C124—C125—C126—C127 −1.3 (3) C224—C225—C226—C227 −1.2 (3)
C128—C125—C126—C127 177.5 (2) C228—C225—C226—C227 178.35 (19)
C125—C126—C127—C122 1.5 (3) C225—C226—C227—C222 0.0 (3)
C123—C122—C127—C126 −0.2 (3) C223—C222—C227—C226 1.2 (3)
P12—C122—C127—C126 −176.92 (14) P22—C222—C227—C226 −171.66 (16)
C136—P12—C129—C134 27.42 (17) C236—P22—C229—C230 −149.74 (14)
C122—P12—C129—C134 133.38 (15) C222—P22—C229—C230 100.68 (15)
Fe1—P12—C129—C134 −105.20 (14) Fe2—P22—C229—C230 −19.72 (17)
C136—P12—C129—C130 −159.89 (14) C236—P22—C229—C234 35.53 (17)
C122—P12—C129—C130 −53.92 (16) C222—P22—C229—C234 −74.06 (16)
Fe1—P12—C129—C130 67.50 (15) Fe2—P22—C229—C234 165.54 (13)
C134—C129—C130—C131 −0.5 (3) C234—C229—C230—C231 0.3 (3)
P12—C129—C130—C131 −173.45 (14) P22—C229—C230—C231 −174.69 (14)
C129—C130—C131—C132 0.8 (3) C229—C230—C231—C232 −0.2 (3)
C130—C131—C132—C133 −0.7 (3) C230—C231—C232—C233 −0.3 (3)
C130—C131—C132—C135 178.10 (19) C230—C231—C232—C235 177.86 (18)
C131—C132—C133—C134 0.2 (3) C231—C232—C233—C234 0.6 (3)
C135—C132—C133—C134 −178.60 (19) C235—C232—C233—C234 −177.55 (18)
C132—C133—C134—C129 0.1 (3) C232—C233—C234—C229 −0.5 (3)
C130—C129—C134—C133 0.0 (3) C230—C229—C234—C233 0.0 (3)
P12—C129—C134—C133 172.80 (14) P22—C229—C234—C233 174.83 (14)
C129—P12—C136—C141 −128.97 (15) C229—P22—C236—C237 −153.01 (14)
C122—P12—C136—C141 123.45 (15) C222—P22—C236—C237 −47.90 (16)
Fe1—P12—C136—C141 1.49 (17) Fe2—P22—C236—C237 73.31 (15)
C129—P12—C136—C137 53.68 (16) C229—P22—C236—C241 38.41 (16)
C122—P12—C136—C137 −53.91 (16) C222—P22—C236—C241 143.52 (15)
Fe1—P12—C136—C137 −175.87 (12) Fe2—P22—C236—C241 −95.27 (14)
C141—C136—C137—C138 0.0 (3) C241—C236—C237—C238 −1.0 (3)
P12—C136—C137—C138 177.39 (14) P22—C236—C237—C238 −169.96 (14)
C136—C137—C138—C139 −0.1 (3) C236—C237—C238—C239 −0.9 (3)
C137—C138—C139—C140 0.4 (3) C237—C238—C239—C240 2.1 (3)
C137—C138—C139—C142 −177.94 (18) C237—C238—C239—C242 −176.25 (17)
C138—C139—C140—C141 −0.5 (3) C238—C239—C240—C241 −1.4 (3)
C142—C139—C140—C141 177.75 (18) C242—C239—C240—C241 176.92 (16)
C137—C136—C141—C140 −0.2 (3) C239—C240—C241—C236 −0.5 (3)
P12—C136—C141—C140 −177.58 (14) C237—C236—C241—C240 1.7 (3)
C139—C140—C141—C136 0.4 (3) P22—C236—C241—C240 170.36 (13)
N21—Fe2—P21—C208 6.36 (8)
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Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: FK2034).

References

  1. Albano, V. G., Araneo, A., Bellon, P. L., Ciani, G. & Manassero, M. (1974). J. Organomet. Chem. 67, 413–422.
  2. Atkinson, F. L., Blackwell, H. E., Brown, N. C., Connelly, N. G., Crossley, J. G., Orpen, A. G., Rieger, A. L. & Rieger, P. H. (1996). J. Chem. Soc. Dalton Trans. pp. 3491–3502.
  3. Bruker (2007). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  4. Eisch, J. J. & King, R. B. (1965). Metal Nitrosyl Derivatives, in Organometallic Syntheses New York: Academic Press.
  5. Li, L., Reginato, N., Urschey, M., Stradiotto, M. & Liarakos, J. D. (2003). Can. J. Chem. 82, 468–475.
  6. Li Kam Wah, H., Postel, M. & Pierrot, M. (1989). Inorg. Chim. Acta, 165, 215–220.
  7. Richter-Addo, G. B. & Legzdins, P. (1992). In Metal Nitrosyls New York: Oxford University Press Inc.
  8. Sheldrick, G. M. (2001). SADABS University of Göttingen, Germany.
  9. Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681100465X/fk2034sup1.cif

e-67-0m331-sup1.cif (53KB, cif)

Structure factors: contains datablocks I. DOI: 10.1107/S160053681100465X/fk2034Isup2.hkl

e-67-0m331-Isup2.hkl (721.8KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography

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