Download citation
Download citation
link to html
The asymmetric unit of the title compound, [Fe(C15H10N3O)2]ClO4·H2O, contains one iron(III) cation chelated by two N-(8-naphth­yl)-2-pyridine-2-carboxamidate ligands via six N atoms, exhibiting an octa­hedral coordination geometry, a perchlorate anion and a water mol­ecule. The Fe-N bond lengths are in the range 1.880 (3)-1.972 (3) Å. Each ligand is planar (r.m.s. deviations = 0.0314 and 0.0282 Å). The dihedral angle between the two ligand planes is 86.55 (1)°. There is a weak inter­molecular hydrogen bond between the water and the perchlorate groups.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807048556/cf2152sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807048556/cf2152Isup2.hkl
Contains datablock I

CCDC reference: 1294011

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.054
  • wR factor = 0.140
  • Data-to-parameter ratio = 13.5

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT245_ALERT_2_B U(iso) H1W Smaller than U(eq) O1W by ... 0.05 AngSq PLAT245_ALERT_2_B U(iso) H2W Smaller than U(eq) O1W by ... 0.05 AngSq PLAT420_ALERT_2_B D-H Without Acceptor O1W - H2W ... ?
Alert level C PLAT230_ALERT_2_C Hirshfeld Test Diff for N4 - C16 .. 5.62 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Fe1 (3) 4.26 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Comment top

Complexes containing carbonyl amine (organic amide) ligands have been the interest of chemists due to their potential applications, such as in catalysis, optics, information storage, medicine, molecular electrochemistry, biochemistry and biological pharmaceuticals (Li et al., 1993; Go et al., 2004). Thus far, N-containing aromatic carbonyl amines have been widely used in dye intermediates, organic synthesis, sensitization materials, functional pigments, adipiodone and acetrizoic acid (An et al., 2000). Pyridine carbonyl amine is also a good ligand in coordination chemistry due to its strong coordination ability and versatile coordination modes, so much attention has been paid to it in recent years (Baroni et al., 1996; Hundal et al., 2002). Here we report the new title complex.

The title compound contains an iron(III) cation chelated by two 2-pyridinecarbonyl-8-aminoquinoline ligands via six N atoms, exhibiting octahedral geometry around the central iron ion (Fig. 1). The Fe—N bond length are in the range 1.880 (3)–1.972 (3) Å. Each ligand is planar (r.m.s. deviations 0.0314 and 0.0282 Å). The dihedral angle between the two ligand planes is 86.55 (1)°. There is a weak intermolecular hydrogen bond between water and perchlorate, contributing to the packing.

Related literature top

For related literature, see: Li et al. (1993); Go et al. (2004); An et al. (2000); Baroni et al. (1996); Hundal et al. (2002).

Experimental top

A mixture of iron trichloride (0.1 mmol) and 2-pyridinecarbonyl-8-aminoquinoline (0.2 mmol) in 25 ml me thanol was refluxed for 2 h and filtered. The filtrate was evaporated naturally in an open flask. Green crystals were obtained after one week in a yield of 12%. Anal. Calc. for C30H22ClFeN6O7: C 53.73, H 2.99, N 12.54%; Found: 53.68, H 3.02, N 12.51%.

Refinement top

The H atoms of the water molecule were located in a difference density map and were refined with distance restraints [H···H = 1.38 (2) Å and O—H = 0.82 (2) Å] and with Uiso(H) = 0.08 Å2. All other H atoms were placed in calculated positions with a C—H bond distance of 0.93 Å and Uiso(H) = 1.2Ueq(C).

Structure description top

Complexes containing carbonyl amine (organic amide) ligands have been the interest of chemists due to their potential applications, such as in catalysis, optics, information storage, medicine, molecular electrochemistry, biochemistry and biological pharmaceuticals (Li et al., 1993; Go et al., 2004). Thus far, N-containing aromatic carbonyl amines have been widely used in dye intermediates, organic synthesis, sensitization materials, functional pigments, adipiodone and acetrizoic acid (An et al., 2000). Pyridine carbonyl amine is also a good ligand in coordination chemistry due to its strong coordination ability and versatile coordination modes, so much attention has been paid to it in recent years (Baroni et al., 1996; Hundal et al., 2002). Here we report the new title complex.

The title compound contains an iron(III) cation chelated by two 2-pyridinecarbonyl-8-aminoquinoline ligands via six N atoms, exhibiting octahedral geometry around the central iron ion (Fig. 1). The Fe—N bond length are in the range 1.880 (3)–1.972 (3) Å. Each ligand is planar (r.m.s. deviations 0.0314 and 0.0282 Å). The dihedral angle between the two ligand planes is 86.55 (1)°. There is a weak intermolecular hydrogen bond between water and perchlorate, contributing to the packing.

For related literature, see: Li et al. (1993); Go et al. (2004); An et al. (2000); Baroni et al. (1996); Hundal et al. (2002).

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of the title structure, drawn with 30% probability displacement ellipsoids.
Bis[N-(8-quinolyl)pyridine-2-carboxamidato]iron(III) perchlorate monohydrate top
Crystal data top
[Fe(C15H10N3O)2]ClO4·H2OZ = 2
Mr = 669.84F(000) = 686
Triclinic, P1Dx = 1.552 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.2452 (10) ÅCell parameters from 5559 reflections
b = 11.944 (2) Åθ = 3.1–26.0°
c = 13.0523 (10) ŵ = 0.68 mm1
α = 95.807 (5)°T = 293 K
β = 90.462 (1)°Block, green
γ = 91.615 (5)°0.42 × 0.26 × 0.22 mm
V = 1433.3 (3) Å3
Data collection top
Bruker APEXII CCD area-detector
diffractometer
5559 independent reflections
Radiation source: fine-focus sealed tube3729 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
φ and ω scansθmax = 26.0°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 011
Tmin = 0.763, Tmax = 0.865k = 1414
13425 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.140H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.092P)2]
where P = (Fo2 + 2Fc2)/3
5559 reflections(Δ/σ)max < 0.001
413 parametersΔρmax = 0.50 e Å3
3 restraintsΔρmin = 0.42 e Å3
Crystal data top
[Fe(C15H10N3O)2]ClO4·H2Oγ = 91.615 (5)°
Mr = 669.84V = 1433.3 (3) Å3
Triclinic, P1Z = 2
a = 9.2452 (10) ÅMo Kα radiation
b = 11.944 (2) ŵ = 0.68 mm1
c = 13.0523 (10) ÅT = 293 K
α = 95.807 (5)°0.42 × 0.26 × 0.22 mm
β = 90.462 (1)°
Data collection top
Bruker APEXII CCD area-detector
diffractometer
5559 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
3729 reflections with I > 2σ(I)
Tmin = 0.763, Tmax = 0.865Rint = 0.022
13425 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0543 restraints
wR(F2) = 0.140H atoms treated by a mixture of independent and constrained refinement
S = 1.00Δρmax = 0.50 e Å3
5559 reflectionsΔρmin = 0.42 e Å3
413 parameters
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
C10.7506 (5)0.3112 (4)0.3721 (3)0.0659 (10)
H1A0.71300.38100.39390.079*
C20.8893 (6)0.2844 (5)0.4060 (4)0.0892 (15)
H2A0.94140.33580.45150.107*
C30.9464 (5)0.1862 (5)0.3735 (4)0.0820 (13)
H3A1.03890.17040.39540.098*
C40.8682 (5)0.1051 (4)0.3056 (3)0.0654 (11)
C50.9158 (5)0.0009 (5)0.2647 (4)0.0792 (13)
H5A1.00730.02340.28260.095*
C60.8324 (6)0.0699 (4)0.2007 (4)0.0796 (14)
H6A0.86770.13920.17510.096*
C70.6920 (5)0.0408 (3)0.1706 (3)0.0628 (10)
H7A0.63610.09050.12610.075*
C80.6395 (4)0.0610 (3)0.2073 (3)0.0499 (8)
C90.7297 (4)0.1362 (3)0.2760 (3)0.0493 (8)
C100.3957 (4)0.0540 (3)0.1333 (3)0.0565 (9)
C110.2748 (4)0.1304 (3)0.1266 (3)0.0558 (9)
C120.1473 (5)0.1020 (4)0.0708 (4)0.0775 (13)
H12A0.13450.03100.03490.093*
C130.0417 (6)0.1792 (5)0.0691 (5)0.0886 (15)
H13A0.04380.16050.03250.106*
C140.0606 (5)0.2840 (4)0.1211 (4)0.0719 (11)
H14A0.01060.33730.11900.086*
C150.1869 (4)0.3094 (3)0.1767 (3)0.0549 (8)
H15A0.19900.37980.21390.066*
C160.3662 (4)0.1163 (4)0.4101 (3)0.0652 (10)
H16A0.39550.05290.36920.078*
C170.2985 (5)0.1049 (5)0.5041 (4)0.0806 (14)
H17A0.28440.03380.52620.097*
C180.2533 (5)0.1969 (5)0.5631 (3)0.0823 (14)
H18A0.20670.18900.62490.099*
C190.2761 (4)0.3008 (4)0.5316 (3)0.0672 (11)
H19A0.24580.36450.57170.081*
C200.3443 (4)0.3107 (3)0.4402 (2)0.0523 (8)
C210.3797 (4)0.4214 (3)0.4006 (3)0.0527 (8)
C220.5049 (4)0.4906 (3)0.2525 (3)0.0466 (7)
C230.4968 (5)0.6065 (3)0.2745 (3)0.0617 (10)
H23A0.44900.63700.33270.074*
C240.5625 (5)0.6769 (3)0.2070 (4)0.0744 (12)
H24A0.55690.75440.22190.089*
C250.6329 (5)0.6370 (3)0.1220 (4)0.0709 (12)
H25A0.67630.68680.08040.085*
C260.6412 (4)0.5202 (3)0.0953 (3)0.0583 (9)
C270.7120 (4)0.4666 (4)0.0094 (3)0.0629 (10)
H27A0.76210.51010.03460.075*
C280.7083 (4)0.3521 (4)0.0105 (3)0.0625 (10)
H28A0.75350.31760.06830.075*
C290.6363 (4)0.2882 (3)0.0567 (3)0.0528 (8)
H29A0.63350.21030.04230.063*
C300.5729 (4)0.4481 (3)0.1621 (3)0.0467 (7)
Cl10.98024 (13)0.38673 (11)0.75442 (12)0.0874 (4)
Fe10.48026 (5)0.25820 (4)0.25203 (3)0.03984 (17)
N10.6730 (3)0.2379 (2)0.3095 (2)0.0500 (7)
N20.5060 (3)0.1068 (2)0.1892 (2)0.0493 (7)
N30.2932 (3)0.2345 (2)0.1783 (2)0.0439 (6)
N40.3889 (3)0.2191 (2)0.3789 (2)0.0478 (6)
N50.4503 (3)0.4062 (2)0.3099 (2)0.0448 (6)
N60.5710 (3)0.3329 (2)0.1409 (2)0.0437 (6)
O10.3877 (4)0.0438 (2)0.0916 (3)0.0865 (10)
O20.3503 (4)0.5108 (3)0.4477 (2)0.0778 (8)
O31.0848 (7)0.4603 (6)0.7251 (5)0.166 (2)
O40.9827 (10)0.2839 (6)0.6934 (8)0.227 (4)
O51.0194 (7)0.3498 (9)0.8547 (6)0.217 (4)
O60.8419 (5)0.4240 (4)0.7667 (4)0.1305 (16)
O1W0.2728 (13)0.8676 (9)0.3076 (14)0.131 (3)
H1W0.205 (4)0.839 (4)0.339 (3)0.080*
H2W0.265 (5)0.846 (5)0.2461 (12)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.065 (2)0.067 (2)0.062 (2)0.0114 (19)0.0079 (19)0.0116 (19)
C20.071 (3)0.103 (4)0.089 (4)0.007 (3)0.023 (2)0.015 (3)
C30.065 (3)0.101 (4)0.081 (3)0.016 (3)0.013 (2)0.010 (3)
C40.068 (2)0.073 (3)0.061 (2)0.024 (2)0.0157 (19)0.029 (2)
C50.072 (3)0.082 (3)0.089 (3)0.028 (2)0.013 (2)0.026 (3)
C60.098 (4)0.065 (3)0.081 (3)0.030 (3)0.033 (3)0.023 (2)
C70.080 (3)0.0421 (18)0.068 (2)0.0120 (17)0.019 (2)0.0127 (17)
C80.065 (2)0.0432 (17)0.0430 (18)0.0080 (15)0.0105 (15)0.0080 (14)
C90.059 (2)0.0482 (18)0.0431 (18)0.0130 (15)0.0152 (14)0.0123 (14)
C100.069 (2)0.0368 (17)0.061 (2)0.0049 (16)0.0072 (18)0.0056 (15)
C110.063 (2)0.0456 (18)0.057 (2)0.0090 (16)0.0050 (16)0.0014 (15)
C120.074 (3)0.067 (3)0.086 (3)0.015 (2)0.007 (2)0.016 (2)
C130.069 (3)0.087 (3)0.106 (4)0.001 (3)0.019 (3)0.005 (3)
C140.058 (2)0.080 (3)0.078 (3)0.005 (2)0.007 (2)0.010 (2)
C150.060 (2)0.053 (2)0.053 (2)0.0063 (16)0.0018 (16)0.0094 (16)
C160.063 (2)0.078 (3)0.058 (2)0.003 (2)0.0010 (18)0.023 (2)
C170.082 (3)0.101 (4)0.064 (3)0.007 (3)0.007 (2)0.035 (3)
C180.075 (3)0.128 (5)0.045 (2)0.004 (3)0.014 (2)0.016 (3)
C190.064 (2)0.096 (3)0.041 (2)0.005 (2)0.0107 (16)0.001 (2)
C200.0500 (19)0.072 (2)0.0333 (16)0.0063 (16)0.0027 (13)0.0014 (15)
C210.055 (2)0.057 (2)0.0434 (18)0.0195 (16)0.0027 (15)0.0150 (15)
C220.0518 (19)0.0366 (16)0.0495 (19)0.0031 (13)0.0073 (14)0.0048 (13)
C230.070 (2)0.0432 (18)0.069 (3)0.0068 (17)0.0058 (19)0.0076 (17)
C240.086 (3)0.0384 (19)0.099 (4)0.0039 (19)0.010 (3)0.010 (2)
C250.075 (3)0.051 (2)0.088 (3)0.015 (2)0.008 (2)0.021 (2)
C260.054 (2)0.053 (2)0.069 (2)0.0122 (17)0.0141 (17)0.0205 (18)
C270.056 (2)0.079 (3)0.057 (2)0.0057 (19)0.0038 (17)0.027 (2)
C280.058 (2)0.081 (3)0.050 (2)0.0023 (19)0.0108 (16)0.0108 (19)
C290.055 (2)0.054 (2)0.0493 (19)0.0042 (15)0.0015 (15)0.0044 (16)
C300.0432 (17)0.0452 (17)0.0511 (19)0.0048 (14)0.0085 (14)0.0033 (14)
Cl10.0700 (7)0.0850 (8)0.1068 (10)0.0213 (6)0.0178 (6)0.0009 (7)
Fe10.0500 (3)0.0338 (2)0.0350 (3)0.00393 (17)0.00660 (17)0.00136 (17)
N10.0540 (16)0.0532 (16)0.0425 (15)0.0015 (13)0.0048 (12)0.0040 (12)
N20.0642 (18)0.0317 (13)0.0509 (16)0.0042 (12)0.0100 (13)0.0018 (11)
N30.0504 (15)0.0390 (13)0.0419 (14)0.0029 (11)0.0076 (11)0.0028 (11)
N40.0561 (16)0.0530 (16)0.0354 (14)0.0044 (13)0.0022 (11)0.0096 (12)
N50.0513 (16)0.0417 (14)0.0408 (14)0.0076 (12)0.0022 (11)0.0013 (11)
N60.0530 (15)0.0378 (13)0.0392 (14)0.0006 (11)0.0033 (11)0.0011 (11)
O10.100 (2)0.0401 (14)0.113 (3)0.0018 (15)0.0040 (19)0.0202 (15)
O20.099 (2)0.0683 (18)0.0624 (17)0.0251 (15)0.0108 (15)0.0191 (14)
O30.149 (5)0.175 (6)0.180 (6)0.043 (4)0.034 (4)0.052 (5)
O40.264 (9)0.114 (5)0.294 (10)0.041 (5)0.111 (7)0.046 (5)
O50.143 (5)0.369 (12)0.157 (6)0.035 (6)0.007 (4)0.110 (7)
O60.107 (3)0.134 (4)0.157 (4)0.057 (3)0.024 (3)0.027 (3)
O1W0.188 (9)0.117 (6)0.088 (6)0.054 (6)0.041 (5)0.008 (5)
Geometric parameters (Å, º) top
C1—N11.327 (5)C18—H18A0.930
C1—C21.410 (6)C19—C201.368 (5)
C1—H1A0.930C19—H19A0.930
C2—C31.332 (7)C20—N41.363 (5)
C2—H2A0.930C20—C211.496 (6)
C3—C41.422 (7)C21—O21.215 (4)
C3—H3A0.930C21—N51.356 (4)
C4—C51.407 (7)C22—C231.389 (5)
C4—C91.406 (6)C22—C301.398 (5)
C5—C61.336 (8)C22—N51.400 (4)
C5—H5A0.930C23—C241.408 (6)
C6—C71.416 (7)C23—H23A0.930
C6—H6A0.930C24—C251.343 (7)
C7—C81.365 (5)C24—H24A0.930
C7—H7A0.930C25—C261.408 (6)
C8—N21.392 (5)C25—H25A0.930
C8—C91.445 (5)C26—C271.409 (6)
C9—N11.368 (5)C26—C301.424 (5)
C10—O11.239 (4)C27—C281.366 (6)
C10—N21.352 (5)C27—H27A0.930
C10—C111.470 (6)C28—C291.381 (5)
C11—N31.359 (4)C28—H28A0.930
C11—C121.396 (6)C29—N61.330 (5)
C12—C131.363 (7)C29—H29A0.930
C12—H12A0.930C30—N61.376 (4)
C13—C141.368 (7)Cl1—O31.371 (5)
C13—H13A0.930Cl1—O61.372 (4)
C14—C151.380 (6)Cl1—O41.395 (7)
C14—H14A0.930Cl1—O51.469 (7)
C15—N31.349 (5)Fe1—N51.880 (3)
C15—H15A0.930Fe1—N21.930 (3)
C16—N41.343 (5)Fe1—N11.959 (3)
C16—C171.400 (6)Fe1—N41.958 (3)
C16—H16A0.930Fe1—N61.960 (3)
C17—C181.355 (8)Fe1—N31.972 (3)
C17—H17A0.930O1W—H1W0.84 (3)
C18—C191.357 (7)O1W—H2W0.82 (3)
N1—C1—C2120.6 (4)C30—C22—N5113.1 (3)
N1—C1—H1A119.7C22—C23—C24118.8 (4)
C2—C1—H1A119.7C22—C23—H23A120.6
C3—C2—C1120.5 (5)C24—C23—H23A120.6
C3—C2—H2A119.7C25—C24—C23122.9 (4)
C1—C2—H2A119.7C25—C24—H24A118.6
C2—C3—C4121.0 (4)C23—C24—H24A118.6
C2—C3—H3A119.5C24—C25—C26120.4 (4)
C4—C3—H3A119.5C24—C25—H25A119.8
C5—C4—C9117.4 (4)C26—C25—H25A119.8
C5—C4—C3126.9 (4)C27—C26—C25126.5 (4)
C9—C4—C3115.7 (4)C27—C26—C30116.3 (3)
C6—C5—C4121.5 (5)C25—C26—C30117.2 (4)
C6—C5—H5A119.3C28—C27—C26121.2 (4)
C4—C5—H5A119.3C28—C27—H27A119.4
C5—C6—C7122.1 (4)C26—C27—H27A119.4
C5—C6—H6A119.0C27—C28—C29118.9 (4)
C7—C6—H6A119.0C27—C28—H28A120.5
C8—C7—C6119.4 (4)C29—C28—H28A120.5
C8—C7—H7A120.3N6—C29—C28123.1 (4)
C6—C7—H7A120.3N6—C29—H29A118.5
C7—C8—N2129.4 (4)C28—C29—H29A118.5
C7—C8—C9118.7 (4)N6—C30—C22116.6 (3)
N2—C8—C9111.8 (3)N6—C30—C26121.5 (3)
N1—C9—C4122.6 (4)C22—C30—C26121.9 (3)
N1—C9—C8116.5 (3)O3—Cl1—O6118.2 (4)
C4—C9—C8120.9 (3)O3—Cl1—O4111.2 (5)
O1—C10—N2128.8 (4)O6—Cl1—O4111.5 (5)
O1—C10—C11120.9 (4)O3—Cl1—O5109.7 (5)
N2—C10—C11110.3 (3)O6—Cl1—O5104.6 (4)
N3—C11—C12120.0 (4)O4—Cl1—O599.8 (6)
N3—C11—C10116.0 (3)N5—Fe1—N2178.08 (13)
C12—C11—C10124.1 (3)N5—Fe1—N198.93 (12)
C13—C12—C11119.5 (4)N2—Fe1—N182.88 (12)
C13—C12—H12A120.3N5—Fe1—N483.05 (12)
C11—C12—H12A120.3N2—Fe1—N497.59 (12)
C12—C13—C14120.4 (4)N1—Fe1—N491.11 (12)
C12—C13—H13A119.8N5—Fe1—N683.80 (11)
C14—C13—H13A119.8N2—Fe1—N695.61 (11)
C13—C14—C15118.9 (4)N1—Fe1—N689.06 (12)
C13—C14—H14A120.5N4—Fe1—N6166.71 (11)
C15—C14—H14A120.5N5—Fe1—N397.17 (12)
N3—C15—C14121.4 (4)N2—Fe1—N381.03 (12)
N3—C15—H15A119.3N1—Fe1—N3163.89 (12)
C14—C15—H15A119.3N4—Fe1—N390.17 (11)
N4—C16—C17119.9 (4)N6—Fe1—N393.34 (11)
N4—C16—H16A120.0C1—N1—C9119.6 (3)
C17—C16—H16A120.0C1—N1—Fe1127.3 (3)
C18—C17—C16120.2 (5)C9—N1—Fe1113.1 (2)
C18—C17—H17A119.9C10—N2—C8125.6 (3)
C16—C17—H17A119.9C10—N2—Fe1118.8 (2)
C19—C18—C17119.8 (4)C8—N2—Fe1115.6 (2)
C19—C18—H18A120.1C15—N3—C11119.7 (3)
C17—C18—H18A120.1C15—N3—Fe1126.5 (2)
C18—C19—C20119.2 (4)C11—N3—Fe1113.8 (2)
C18—C19—H19A120.4C16—N4—C20118.8 (3)
C20—C19—H19A120.4C16—N4—Fe1128.1 (3)
N4—C20—C19122.0 (4)C20—N4—Fe1113.1 (2)
N4—C20—C21114.7 (3)C21—N5—C22126.6 (3)
C19—C20—C21123.4 (4)C21—N5—Fe1118.4 (2)
O2—C21—N5126.8 (4)C22—N5—Fe1115.0 (2)
O2—C21—C20122.5 (3)C29—N6—C30118.9 (3)
N5—C21—C20110.7 (3)C29—N6—Fe1129.5 (2)
C23—C22—C30118.8 (3)C30—N6—Fe1111.4 (2)
C23—C22—N5128.1 (3)H1W—O1W—H2W109 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O4i0.84 (3)2.25 (4)2.934 (12)139 (4)
Symmetry code: (i) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formula[Fe(C15H10N3O)2]ClO4·H2O
Mr669.84
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.2452 (10), 11.944 (2), 13.0523 (10)
α, β, γ (°)95.807 (5), 90.462 (1), 91.615 (5)
V3)1433.3 (3)
Z2
Radiation typeMo Kα
µ (mm1)0.68
Crystal size (mm)0.42 × 0.26 × 0.22
Data collection
DiffractometerBruker APEXII CCD area-detector
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.763, 0.865
No. of measured, independent and
observed [I > 2σ(I)] reflections
13425, 5559, 3729
Rint0.022
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.054, 0.140, 1.00
No. of reflections5559
No. of parameters413
No. of restraints3
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.50, 0.42

Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W···O4i0.84 (3)2.25 (4)2.934 (12)139 (4)
Symmetry code: (i) x+1, y+1, z+1.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds