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The title compound, [FeCl2(C27H34N4O)]·CH3CN, was readily synthesized from the reaction of FeCl2·4H2O and N-(2,6-diiso­propyl­phenyl)-2-[(di-2-pyridyl­methyl)­amino]­ethan­amide in THF. The iron(II) metal center is in an octahedral geometry. There is an intermolecular hydrogen bond between the amide H and one chlorine of a neighboring complex.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680301345X/ac6045sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680301345X/ac6045Isup2.hkl
Contains datablock I

CCDC reference: 217385

Key indicators

  • Single-crystal X-ray study
  • T = 91 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.029
  • wR factor = 0.075
  • Data-to-parameter ratio = 26.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry

General Notes

REFLT_03 From the CIF: _diffrn_reflns_theta_max 31.48 From the CIF: _reflns_number_total 9258 Count of symmetry unique reflns 5409 Completeness (_total/calc) 171.16% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3849 Fraction of Friedel pairs measured 0.712 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.

Comment top

Iron coordination complexes have been studied as small molecule analogs of metalloproteins (Marlin et al., 2002; Rowland et al., 2001; Sams et al., 2001) and recently have gained considerable interest as catalysts for atom transfer reactions and controlled `living' radical polymerizations (Kamigaito et al., 2001; Matyjaszewski & Xia, 2001; Patten & Matyjaszewski, 1999). During the course of our studies on using monoanionic tetradentate ligands to prepare copper(I)–based atom transfer radical polymerization catalysts, we investigated the complexation of a bis(picolyl)amine-based ligand to iron(II) (Kobayashi et al., 1998; Niklas et al., 2000, 2001). The addition of FeCl2·4H2O to a THF solution of N-(2,6-diisopropylphenyl)-2-[(di-2-pyridylmethyl)amino]ethanamide formed the complex. An IR spectrum showed bands corresponding to the presence of the amide N—H group (3410 cm−1) and the amide carbonyl group (1607 cm−1).

The structure of the complex is monomeric with one molecule of cocrystallized acetonitrile, and the iron(II) center is in near octahedral geometry, taking into account the constraints of the tethers between the nitrogen atoms. The amide group is hydrogen bonded to a chlorine atom of the neighboring complex to form chains of complexes throughout the crystal.

Experimental top

All chemicals were purchased from Acros and used without further purification. Acetonitrile was dried using appropriate procedures, and the recrystallization was performed using standard Schlenk techniques. The synthesis of ligand N-(2,6-diisopropylphenyl)-2-[(di-2-pyridylmethyl)amino]ethanamide will be described in a subsequent publication (Troeltzsch et al., 2003). The ligand (1.02 g, 2.37 mmol) was dissolved in 25 ml of THF, and then 0.472 g (2.38 mmol) of FeCl2·4H2O was added. The solution was stirred and then concentrated to dryness. The solid was dissolved in boiling, dry acetonitrile, and upon cooling amber needles formed suitable for X-ray analysis [m.p. 446 K (decomposition)]. Elemental composition, calculated: C 58.21, H 6.23, N 11.70%; found: C 57.09, H 6.14, N 11.69%. IR (Thin film, NaCl plates) ν (cm-1): 3410 (broad), 1607 (s), 1563 (m).

Refinement top

H atoms were placed in idealized positions and refined using a model whereby the H atom was riding on the bonded carbon with an Uiso value equal to 1.2 (1.5 for methyl H) times the Ueq value of the bonded carbon.

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Sheldrick, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. View of (I), showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level.
(I) top
Crystal data top
[FeCl2(C27H34N4O)]·CH3CNDx = 1.346 Mg m3
Mr = 598.39Melting point: 446 K
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 7272 reflections
a = 13.1579 (4) Åθ = 2.5–31.4°
b = 14.2791 (5) ŵ = 0.72 mm1
c = 15.7210 (5) ÅT = 91 K
V = 2953.71 (17) Å3Needle, brown
Z = 40.27 × 0.27 × 0.22 mm
F(000) = 1256
Data collection top
Bruker SMART 1000
diffractometer
9258 independent reflections
Radiation source: normal-focus sealed tube8527 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
Detector resolution: 8.2 pixels mm-1θmax = 31.5°, θmin = 1.9°
ω scansh = 1919
Absorption correction: multi-scan
(SADABS; Sheldrick, 2000)
k = 2020
Tmin = 0.829, Tmax = 0.857l = 2222
27291 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.029H-atom parameters constrained
wR(F2) = 0.075 w = 1/[σ2(Fo2) + (0.0464P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.001
9258 reflectionsΔρmax = 0.53 e Å3
348 parametersΔρmin = 0.22 e Å3
0 restraintsAbsolute structure: 3928 Friedel pairs were measured for determination of the Flack parameter Flack (1983).
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.015 (8)
Crystal data top
[FeCl2(C27H34N4O)]·CH3CNV = 2953.71 (17) Å3
Mr = 598.39Z = 4
Orthorhombic, P212121Mo Kα radiation
a = 13.1579 (4) ŵ = 0.72 mm1
b = 14.2791 (5) ÅT = 91 K
c = 15.7210 (5) Å0.27 × 0.27 × 0.22 mm
Data collection top
Bruker SMART 1000
diffractometer
9258 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2000)
8527 reflections with I > 2σ(I)
Tmin = 0.829, Tmax = 0.857Rint = 0.023
27291 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.029H-atom parameters constrained
wR(F2) = 0.075Δρmax = 0.53 e Å3
S = 1.07Δρmin = 0.22 e Å3
9258 reflectionsAbsolute structure: 3928 Friedel pairs were measured for determination of the Flack parameter Flack (1983).
348 parametersAbsolute structure parameter: 0.015 (8)
0 restraints
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)

are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based

on F, with F set to zero for negative F2. The threshold expression of

F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.713985 (15)0.972432 (13)0.944912 (12)0.01420 (5)
Cl10.75938 (3)0.85357 (2)1.03967 (2)0.01847 (7)
Cl20.58245 (3)1.05705 (2)1.03564 (2)0.01755 (7)
O10.80662 (8)0.90524 (8)0.84702 (7)0.0181 (2)
N10.82842 (10)1.07675 (9)0.97473 (9)0.0192 (3)
N20.58382 (11)0.92640 (9)0.87390 (8)0.0197 (3)
N30.69149 (10)1.08964 (9)0.84539 (9)0.0184 (2)
N40.86896 (10)0.85919 (9)0.71966 (8)0.0161 (2)
H4A0.88240.87730.66730.019*
C10.91379 (13)1.05968 (11)1.01947 (11)0.0227 (3)
H10.92111.00051.04650.027*
C20.99117 (14)1.12454 (13)1.02774 (12)0.0281 (4)
H21.05051.11021.05960.034*
C30.98032 (15)1.21080 (14)0.98872 (13)0.0320 (4)
H31.03291.25620.99240.038*
C40.89223 (13)1.23014 (11)0.94435 (12)0.0268 (3)
H40.88291.28940.91800.032*
C50.81731 (12)1.16169 (10)0.93884 (11)0.0211 (3)
C60.71766 (13)1.17651 (10)0.89280 (10)0.0213 (3)
H6A0.66331.19130.93430.026*
H6B0.72381.22970.85280.026*
C70.58364 (13)1.08689 (12)0.82105 (11)0.0228 (3)
H7A0.57571.11530.76400.027*
H7B0.54381.12490.86190.027*
C80.54166 (12)0.98849 (11)0.81940 (10)0.0200 (3)
C90.45969 (13)0.96431 (13)0.76778 (11)0.0264 (3)
H90.43351.00750.72740.032*
C100.41723 (14)0.87638 (14)0.77653 (12)0.0303 (4)
H100.36070.85880.74260.036*
C110.45758 (14)0.81370 (13)0.83526 (12)0.0291 (4)
H110.42780.75380.84360.035*
C120.54264 (13)0.84118 (12)0.88140 (11)0.0240 (3)
H120.57260.79780.91970.029*
C130.76084 (13)1.08697 (11)0.77053 (10)0.0203 (3)
H13A0.83081.10050.79020.024*
H13B0.74091.13760.73090.024*
C140.76199 (12)0.99529 (11)0.72210 (10)0.0201 (3)
H14A0.69110.97600.71030.024*
H14B0.79631.00510.66680.024*
C150.81530 (11)0.91727 (10)0.76933 (9)0.0161 (3)
C160.90592 (11)0.76933 (10)0.74647 (9)0.0151 (3)
C170.98788 (11)0.76245 (10)0.80272 (10)0.0167 (3)
C181.02026 (12)0.67263 (11)0.82660 (10)0.0191 (3)
H181.07500.66610.86550.023*
C190.97355 (13)0.59347 (11)0.79423 (11)0.0212 (3)
H190.99630.53310.81120.025*
C200.89360 (12)0.60174 (11)0.73706 (10)0.0209 (3)
H200.86310.54690.71430.025*
C210.85729 (12)0.68977 (10)0.71252 (10)0.0176 (3)
C221.04354 (12)0.84742 (10)0.83756 (10)0.0189 (3)
H221.00950.90500.81510.023*
C231.03971 (14)0.85060 (12)0.93484 (11)0.0265 (3)
H23A0.96890.84670.95380.040*
H23B1.06960.90940.95490.040*
H23C1.07820.79770.95810.040*
C241.15450 (12)0.84763 (12)0.80676 (11)0.0229 (3)
H24A1.18770.78920.82420.034*
H24B1.19050.90100.83190.034*
H24C1.15600.85280.74460.034*
C250.76486 (12)0.70013 (11)0.65500 (10)0.0213 (3)
H250.77770.75380.61560.026*
C260.74310 (16)0.61331 (13)0.60082 (12)0.0307 (4)
H26A0.80390.59700.56800.046*
H26B0.68680.62650.56180.046*
H26C0.72470.56090.63800.046*
C270.67034 (13)0.72393 (13)0.70881 (13)0.0278 (4)
H27A0.65430.67110.74630.042*
H27B0.61250.73610.67110.042*
H27C0.68410.77970.74320.042*
N50.71807 (16)0.47898 (16)0.88458 (12)0.0502 (5)
C280.76392 (16)0.53398 (17)0.92082 (12)0.0382 (5)
C290.82307 (18)0.60265 (18)0.96872 (16)0.0486 (6)
H29A0.79160.61261.02450.073*
H29B0.82480.66200.93740.073*
H29C0.89250.57940.97640.073*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.01621 (9)0.01389 (8)0.01250 (9)0.00141 (7)0.00049 (7)0.00111 (7)
Cl10.02268 (16)0.01662 (13)0.01612 (15)0.00270 (12)0.00246 (12)0.00357 (12)
Cl20.01952 (16)0.01894 (14)0.01420 (15)0.00279 (12)0.00081 (12)0.00129 (11)
O10.0206 (5)0.0199 (5)0.0138 (5)0.0044 (4)0.0023 (4)0.0022 (4)
N10.0192 (6)0.0167 (6)0.0219 (6)0.0001 (5)0.0024 (5)0.0004 (5)
N20.0197 (6)0.0218 (6)0.0176 (6)0.0014 (5)0.0015 (5)0.0031 (5)
N30.0198 (6)0.0179 (5)0.0174 (6)0.0038 (5)0.0024 (5)0.0012 (5)
N40.0202 (6)0.0153 (5)0.0126 (5)0.0035 (5)0.0012 (4)0.0024 (4)
C10.0217 (7)0.0224 (7)0.0242 (7)0.0003 (6)0.0013 (6)0.0028 (6)
C20.0237 (8)0.0321 (9)0.0285 (9)0.0045 (6)0.0031 (6)0.0041 (7)
C30.0332 (10)0.0311 (9)0.0318 (9)0.0123 (8)0.0009 (8)0.0019 (7)
C40.0336 (9)0.0188 (7)0.0279 (8)0.0055 (6)0.0024 (7)0.0014 (7)
C50.0228 (7)0.0180 (6)0.0226 (7)0.0000 (5)0.0043 (6)0.0011 (6)
C60.0224 (7)0.0162 (6)0.0251 (7)0.0009 (6)0.0029 (6)0.0028 (5)
C70.0236 (8)0.0225 (7)0.0223 (8)0.0058 (6)0.0045 (6)0.0003 (6)
C80.0166 (6)0.0245 (7)0.0190 (7)0.0026 (6)0.0007 (5)0.0020 (6)
C90.0207 (7)0.0347 (9)0.0238 (8)0.0050 (7)0.0045 (6)0.0052 (7)
C100.0186 (7)0.0406 (10)0.0317 (9)0.0007 (7)0.0028 (7)0.0106 (7)
C110.0271 (8)0.0292 (8)0.0309 (9)0.0078 (7)0.0046 (7)0.0084 (7)
C120.0233 (8)0.0271 (8)0.0214 (8)0.0019 (6)0.0016 (6)0.0039 (6)
C130.0238 (8)0.0179 (6)0.0192 (7)0.0007 (5)0.0033 (6)0.0025 (5)
C140.0234 (8)0.0202 (6)0.0166 (6)0.0054 (5)0.0016 (5)0.0024 (5)
C150.0158 (6)0.0146 (6)0.0179 (7)0.0009 (5)0.0014 (5)0.0013 (5)
C160.0156 (6)0.0144 (6)0.0153 (6)0.0035 (5)0.0024 (5)0.0015 (5)
C170.0159 (7)0.0159 (6)0.0181 (7)0.0013 (5)0.0016 (5)0.0007 (5)
C180.0177 (7)0.0190 (7)0.0207 (7)0.0016 (5)0.0012 (6)0.0021 (5)
C190.0243 (8)0.0140 (6)0.0253 (8)0.0018 (6)0.0005 (6)0.0019 (5)
C200.0227 (7)0.0156 (7)0.0244 (8)0.0006 (6)0.0009 (6)0.0004 (6)
C210.0182 (7)0.0175 (6)0.0170 (7)0.0007 (5)0.0006 (5)0.0001 (5)
C220.0173 (6)0.0156 (6)0.0238 (7)0.0009 (5)0.0016 (5)0.0001 (5)
C230.0280 (8)0.0273 (8)0.0241 (8)0.0008 (6)0.0000 (6)0.0068 (7)
C240.0194 (7)0.0207 (7)0.0286 (8)0.0015 (6)0.0005 (6)0.0013 (6)
C250.0227 (8)0.0199 (7)0.0211 (7)0.0006 (6)0.0036 (6)0.0012 (5)
C260.0344 (9)0.0288 (8)0.0290 (9)0.0006 (7)0.0091 (7)0.0071 (7)
C270.0199 (8)0.0280 (8)0.0353 (10)0.0004 (6)0.0031 (7)0.0046 (7)
N50.0455 (11)0.0742 (14)0.0308 (8)0.0239 (11)0.0039 (8)0.0035 (9)
C280.0319 (10)0.0568 (13)0.0258 (8)0.0118 (9)0.0038 (7)0.0025 (8)
C290.0427 (12)0.0600 (14)0.0431 (13)0.0189 (11)0.0141 (10)0.0188 (11)
Geometric parameters (Å, º) top
Fe1—N22.1475 (14)C13—H13A0.9900
Fe1—N12.1693 (13)C13—H13B0.9900
Fe1—O12.1850 (11)C14—C151.512 (2)
Fe1—N32.3101 (13)C14—H14A0.9900
Fe1—Cl12.3360 (4)C14—H14B0.9900
Fe1—Cl22.5474 (4)C16—C171.398 (2)
O1—C151.2387 (18)C16—C211.409 (2)
N1—C51.3455 (19)C17—C181.403 (2)
N1—C11.347 (2)C17—C221.519 (2)
N2—C121.337 (2)C18—C191.384 (2)
N2—C81.352 (2)C18—H180.9500
N3—C71.470 (2)C19—C201.389 (2)
N3—C61.487 (2)C19—H190.9500
N3—C131.490 (2)C20—C211.399 (2)
N4—C151.3403 (18)C20—H200.9500
N4—C161.4354 (18)C21—C251.523 (2)
N4—H4A0.8800C22—C231.531 (2)
C1—C21.383 (2)C22—C241.538 (2)
C1—H10.9500C22—H221.0000
C2—C31.383 (3)C23—H23A0.9800
C2—H20.9500C23—H23B0.9800
C3—C41.381 (3)C23—H23C0.9800
C3—H30.9500C24—H24A0.9800
C4—C51.391 (2)C24—H24B0.9800
C4—H40.9500C24—H24C0.9800
C5—C61.513 (2)C25—C261.531 (2)
C6—H6A0.9900C25—C271.542 (2)
C6—H6B0.9900C25—H251.0000
C7—C81.510 (2)C26—H26A0.9800
C7—H7A0.9900C26—H26B0.9800
C7—H7B0.9900C26—H26C0.9800
C8—C91.393 (2)C27—H27A0.9800
C9—C101.381 (3)C27—H27B0.9800
C9—H90.9500C27—H27C0.9800
C10—C111.391 (3)N5—C281.142 (3)
C10—H100.9500C28—C291.461 (3)
C11—C121.390 (2)C29—H29A0.9800
C11—H110.9500C29—H29B0.9800
C12—H120.9500C29—H29C0.9800
C13—C141.514 (2)
N2—Fe1—N1151.17 (5)C14—C13—H13A108.5
N2—Fe1—O186.81 (5)N3—C13—H13B108.5
N1—Fe1—O193.81 (5)C14—C13—H13B108.5
N2—Fe1—N376.56 (5)H13A—C13—H13B107.5
N1—Fe1—N374.80 (5)C15—C14—C13113.25 (13)
O1—Fe1—N384.99 (4)C15—C14—H14A108.9
N2—Fe1—Cl1108.24 (4)C13—C14—H14A108.9
N1—Fe1—Cl1100.58 (4)C15—C14—H14B108.9
O1—Fe1—Cl189.28 (3)C13—C14—H14B108.9
N3—Fe1—Cl1172.34 (3)H14A—C14—H14B107.7
N2—Fe1—Cl283.94 (4)O1—C15—N4122.50 (13)
N1—Fe1—Cl291.43 (4)O1—C15—C14122.95 (13)
O1—Fe1—Cl2168.98 (3)N4—C15—C14114.48 (13)
N3—Fe1—Cl287.05 (3)C17—C16—C21122.23 (13)
Cl1—Fe1—Cl299.280 (13)C17—C16—N4120.66 (13)
C15—O1—Fe1133.24 (10)C21—C16—N4117.10 (13)
C5—N1—C1118.20 (14)C16—C17—C18117.90 (14)
C5—N1—Fe1116.93 (11)C16—C17—C22122.93 (13)
C1—N1—Fe1124.55 (10)C18—C17—C22119.16 (13)
C12—N2—C8119.10 (14)C19—C18—C17120.91 (14)
C12—N2—Fe1123.77 (11)C19—C18—H18119.5
C8—N2—Fe1117.13 (11)C17—C18—H18119.5
C7—N3—C6112.09 (12)C18—C19—C20120.33 (14)
C7—N3—C13112.63 (13)C18—C19—H19119.8
C6—N3—C13105.99 (12)C20—C19—H19119.8
C7—N3—Fe1106.29 (10)C19—C20—C21120.91 (14)
C6—N3—Fe1103.60 (9)C19—C20—H20119.5
C13—N3—Fe1115.98 (9)C21—C20—H20119.5
C15—N4—C16124.09 (12)C20—C21—C16117.70 (14)
C15—N4—H4A118.0C20—C21—C25121.60 (14)
C16—N4—H4A118.0C16—C21—C25120.62 (13)
N1—C1—C2122.81 (16)C17—C22—C23111.59 (13)
N1—C1—H1118.6C17—C22—C24110.22 (13)
C2—C1—H1118.6C23—C22—C24110.22 (14)
C1—C2—C3118.60 (17)C17—C22—H22108.2
C1—C2—H2120.7C23—C22—H22108.2
C3—C2—H2120.7C24—C22—H22108.2
C4—C3—C2119.25 (17)C22—C23—H23A109.5
C4—C3—H3120.4C22—C23—H23B109.5
C2—C3—H3120.4H23A—C23—H23B109.5
C3—C4—C5119.07 (16)C22—C23—H23C109.5
C3—C4—H4120.5H23A—C23—H23C109.5
C5—C4—H4120.5H23B—C23—H23C109.5
N1—C5—C4122.02 (16)C22—C24—H24A109.5
N1—C5—C6114.89 (13)C22—C24—H24B109.5
C4—C5—C6123.08 (14)H24A—C24—H24B109.5
N3—C6—C5108.89 (12)C22—C24—H24C109.5
N3—C6—H6A109.9H24A—C24—H24C109.5
C5—C6—H6A109.9H24B—C24—H24C109.5
N3—C6—H6B109.9C21—C25—C26113.64 (14)
C5—C6—H6B109.9C21—C25—C27109.87 (13)
H6A—C6—H6B108.3C26—C25—C27109.44 (14)
N3—C7—C8112.48 (13)C21—C25—H25107.9
N3—C7—H7A109.1C26—C25—H25107.9
C8—C7—H7A109.1C27—C25—H25107.9
N3—C7—H7B109.1C25—C26—H26A109.5
C8—C7—H7B109.1C25—C26—H26B109.5
H7A—C7—H7B107.8H26A—C26—H26B109.5
N2—C8—C9121.62 (15)C25—C26—H26C109.5
N2—C8—C7116.69 (13)H26A—C26—H26C109.5
C9—C8—C7121.59 (15)H26B—C26—H26C109.5
C10—C9—C8118.71 (17)C25—C27—H27A109.5
C10—C9—H9120.6C25—C27—H27B109.5
C8—C9—H9120.6H27A—C27—H27B109.5
C9—C10—C11119.78 (16)C25—C27—H27C109.5
C9—C10—H10120.1H27A—C27—H27C109.5
C11—C10—H10120.1H27B—C27—H27C109.5
C12—C11—C10118.16 (17)N5—C28—C29178.6 (3)
C12—C11—H11120.9C28—C29—H29A109.5
C10—C11—H11120.9C28—C29—H29B109.5
N2—C12—C11122.48 (17)H29A—C29—H29B109.5
N2—C12—H12118.8C28—C29—H29C109.5
C11—C12—H12118.8H29A—C29—H29C109.5
N3—C13—C14115.18 (13)H29B—C29—H29C109.5
N3—C13—H13A108.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4A···Cl2i0.882.323.1951 (13)173
Symmetry code: (i) x+3/2, y+2, z1/2.

Experimental details

Crystal data
Chemical formula[FeCl2(C27H34N4O)]·CH3CN
Mr598.39
Crystal system, space groupOrthorhombic, P212121
Temperature (K)91
a, b, c (Å)13.1579 (4), 14.2791 (5), 15.7210 (5)
V3)2953.71 (17)
Z4
Radiation typeMo Kα
µ (mm1)0.72
Crystal size (mm)0.27 × 0.27 × 0.22
Data collection
DiffractometerBruker SMART 1000
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2000)
Tmin, Tmax0.829, 0.857
No. of measured, independent and
observed [I > 2σ(I)] reflections
27291, 9258, 8527
Rint0.023
(sin θ/λ)max1)0.735
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.075, 1.07
No. of reflections9258
No. of parameters348
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.53, 0.22
Absolute structure3928 Friedel pairs were measured for determination of the Flack parameter Flack (1983).
Absolute structure parameter0.015 (8)

Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL (Sheldrick, 1994), SHELXL97.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4A···Cl2i0.882.323.1951 (13)173
Symmetry code: (i) x+3/2, y+2, z1/2.
 

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