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In the title compound, [Fe(C12H8N2)3](NO3)3·H2O, the Fe atom lies on a twofold rotation axis and is coordinated by three planar 1,10-phenanthroline ligands in a slightly distorted octahedral environment. One nitrate anion and the disordered water mol­ecule also lie on twofold rotation axes. The crystal structure is stabilized by partial stacking and hydrogen-bonding interactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804027345/cf6374sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804027345/cf6374Isup2.hkl
Contains datablock I

CCDC reference: 258663

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.043
  • wR factor = 0.123
  • Data-to-parameter ratio = 15.1

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.732 0.904 Tmin' and Tmax expected: 0.899 0.902 RR' = 0.812 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.81 PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N4 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N5
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku/MSC & Rigaku Corporation, 2004); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC & Rigaku Corporation, 2004, 2004)'; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: CrystalStructure.

Tris(1,10-phenanthroline-κ2N,N')iron(III) trinitrate monohydrate top
Crystal data top
[Fe(C12H8N2)3](NO3)3·H2OF(000) = 1546.00
Mr = 800.50Dx = 1.553 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -c_2ycCell parameters from 12716 reflections
a = 10.769 (8) Åθ = 3.1–27.4°
b = 24.58 (2) ŵ = 0.52 mm1
c = 13.274 (12) ÅT = 296 K
β = 103.00 (3)°Block, brown
V = 3423 (5) Å30.20 × 0.20 × 0.20 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
2512 reflections with I > 2σ(I)
Detector resolution: 10.00 pixels mm-1Rint = 0.024
ω scansθmax = 27.4°
Absorption correction: multi-scan
(Higashi, 1995).
h = 1213
Tmin = 0.732, Tmax = 0.904k = 3131
16262 measured reflectionsl = 1717
3869 independent reflections
Refinement top
Refinement on F2H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.043 w = 1/[σ2(Fo2) + (0.0811P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.123(Δ/σ)max < 0.001
S = 1.02Δρmax = 0.71 e Å3
3869 reflectionsΔρmin = 0.49 e Å3
256 parameters
Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Fe10.00000.12256 (2)0.25000.0277 (1)
O10.1505 (3)0.4614 (1)0.1272 (2)0.1078 (9)
O20.1426 (3)0.3892 (1)0.2167 (2)0.124 (1)
O30.2222 (3)0.3865 (1)0.0849 (3)0.1078 (9)
O40.4204 (4)0.1109 (3)0.1971 (3)0.219 (3)
O50.50000.1821 (2)0.25000.172 (3)
O60.00000.4926 (2)0.25000.190 (3)
N10.1591 (1)0.12416 (6)0.1397 (1)0.0300 (3)
N20.0521 (1)0.17956 (7)0.1636 (1)0.0300 (3)
N30.0640 (1)0.06271 (7)0.1771 (1)0.0322 (4)
N40.1731 (3)0.4115 (1)0.1436 (2)0.0791 (8)
N50.50000.1343 (2)0.25000.0672 (9)
C10.2660 (2)0.09459 (9)0.1290 (2)0.0390 (5)
C20.3674 (2)0.0992 (1)0.0422 (2)0.0446 (5)
C30.3597 (2)0.1342 (1)0.0360 (2)0.0430 (5)
C40.2491 (2)0.16589 (9)0.0278 (2)0.0361 (4)
C50.1518 (2)0.15917 (8)0.0619 (1)0.0300 (4)
C60.2282 (2)0.2034 (1)0.1046 (2)0.0442 (5)
C70.1208 (2)0.2341 (1)0.0901 (2)0.0445 (5)
C80.0222 (2)0.22913 (8)0.0018 (2)0.0363 (4)
C90.0373 (2)0.19028 (8)0.0758 (1)0.0301 (4)
C100.0893 (2)0.26122 (9)0.0249 (2)0.0440 (5)
C110.1782 (2)0.2509 (1)0.1135 (2)0.0457 (5)
C120.1589 (2)0.20942 (9)0.1797 (2)0.0377 (5)
C130.1325 (2)0.0641 (1)0.1044 (2)0.0422 (5)
C140.1728 (2)0.0169 (1)0.0629 (2)0.0521 (6)
C150.1426 (2)0.0325 (1)0.0953 (2)0.0542 (6)
C160.0707 (2)0.03630 (9)0.1719 (2)0.0446 (5)
C170.0349 (2)0.01282 (8)0.2101 (2)0.0336 (4)
C180.0333 (3)0.0860 (1)0.2124 (2)0.0595 (7)
H10.27310.07020.18100.047*
H20.44030.07820.03790.053*
H30.42670.13710.09390.052*
H40.28960.20700.16590.053*
H50.11110.25870.14090.053*
H60.10200.28890.01950.053*
H70.25220.27160.12980.055*
H80.22310.20210.23780.045*
H90.15380.09770.08090.051*
H100.22050.01950.01280.063*
H110.16920.06390.06720.065*
H120.05500.11900.18660.071*
H130.07300.47800.25100.285*0.5
H140.00000.52900.25000.285*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0319 (2)0.0267 (2)0.0247 (2)0.00000.0069 (1)0.0000
O10.137 (2)0.080 (2)0.106 (2)0.008 (2)0.026 (2)0.015 (2)
O20.118 (2)0.167 (3)0.082 (2)0.059 (2)0.010 (2)0.045 (2)
O30.136 (3)0.084 (2)0.103 (2)0.027 (2)0.026 (2)0.006 (2)
O40.141 (3)0.395 (7)0.139 (4)0.152 (4)0.070 (3)0.107 (4)
O50.275 (7)0.085 (3)0.213 (6)0.00000.175 (6)0.0000
O60.175 (5)0.093 (4)0.337 (9)0.00000.132 (6)0.0000
N10.0331 (8)0.0293 (9)0.0282 (8)0.0004 (6)0.0081 (6)0.0026 (7)
N20.0334 (8)0.0287 (9)0.0283 (8)0.0011 (6)0.0078 (7)0.0016 (7)
N30.0357 (9)0.032 (1)0.0287 (9)0.0008 (7)0.0062 (7)0.0013 (7)
N40.066 (2)0.097 (2)0.065 (2)0.030 (2)0.005 (1)0.013 (2)
N50.061 (2)0.079 (3)0.071 (2)0.00000.035 (2)0.0000
C10.038 (1)0.043 (1)0.037 (1)0.0060 (9)0.0084 (9)0.000 (1)
C20.035 (1)0.053 (1)0.044 (1)0.0083 (9)0.0049 (9)0.005 (1)
C30.037 (1)0.049 (1)0.038 (1)0.0032 (9)0.0009 (9)0.008 (1)
C40.042 (1)0.035 (1)0.030 (1)0.0072 (8)0.0048 (8)0.0037 (9)
C50.0351 (9)0.028 (1)0.028 (1)0.0043 (7)0.0081 (8)0.0030 (8)
C60.055 (1)0.043 (1)0.030 (1)0.010 (1)0.0001 (9)0.004 (1)
C70.057 (1)0.041 (1)0.036 (1)0.009 (1)0.011 (1)0.010 (1)
C80.046 (1)0.031 (1)0.034 (1)0.0046 (9)0.0150 (9)0.0031 (9)
C90.037 (1)0.026 (1)0.029 (1)0.0032 (7)0.0102 (8)0.0009 (8)
C100.054 (1)0.036 (1)0.047 (1)0.001 (1)0.022 (1)0.008 (1)
C110.047 (1)0.045 (1)0.048 (1)0.012 (1)0.016 (1)0.000 (1)
C120.039 (1)0.038 (1)0.036 (1)0.0069 (9)0.0079 (9)0.0008 (9)
C130.048 (1)0.047 (1)0.035 (1)0.002 (1)0.0158 (9)0.005 (1)
C140.055 (1)0.057 (2)0.049 (1)0.006 (1)0.022 (1)0.011 (1)
C150.059 (1)0.046 (1)0.060 (2)0.011 (1)0.017 (1)0.017 (1)
C160.044 (1)0.034 (1)0.052 (1)0.0049 (9)0.003 (1)0.007 (1)
C170.034 (1)0.031 (1)0.034 (1)0.0001 (8)0.0029 (8)0.0030 (9)
C180.064 (2)0.032 (1)0.082 (2)0.004 (1)0.014 (1)0.007 (1)
Geometric parameters (Å, º) top
Fe1—N11.988 (1)C3—H30.93
Fe1—N1i1.988 (1)C4—C51.408 (2)
Fe1—N21.971 (2)C4—C61.430 (3)
Fe1—N2i1.971 (2)C5—C91.427 (3)
Fe1—N31.968 (2)C6—C71.357 (3)
Fe1—N3i1.968 (2)C6—H40.93
O1—N41.259 (5)C7—C81.431 (3)
O2—N41.222 (5)C7—H50.93
O3—N41.204 (5)C8—C91.406 (3)
O4—N51.134 (5)C8—C101.412 (3)
O5—N51.174 (7)C10—C111.363 (3)
O6—H130.87C10—H60.93
O6—H13i0.87C11—C121.391 (3)
O6—H140.89C11—H70.93
N1—C11.341 (3)C12—H80.93
N1—C51.361 (3)C13—C141.394 (4)
N2—C91.360 (2)C13—H90.93
N2—C121.341 (3)C14—C151.353 (4)
N3—C131.340 (3)C14—H100.93
N3—C171.362 (3)C15—C161.414 (4)
N5—O4ii1.134 (5)C15—H110.93
C1—C21.403 (3)C16—C171.397 (3)
C1—H10.93C16—C181.428 (4)
C2—C31.366 (3)C17—C17i1.430 (3)
C2—H20.93C18—C18i1.353 (5)
C3—C41.406 (3)C18—H120.93
N1—Fe1—N1i177.73 (7)C5—C4—C6118.2 (2)
N1—Fe1—N282.43 (6)C6—C4—C3124.6 (2)
N1—Fe1—N2i95.95 (6)C9—C5—N1115.9 (1)
N1—Fe1—N389.53 (6)C9—C5—C4120.2 (2)
N1—Fe1—N3i92.17 (6)C7—C6—C4121.5 (2)
N1i—Fe1—N295.95 (6)C7—C6—H4119.2
N1i—Fe1—N2i82.43 (6)H4—C6—C4119.2
N1i—Fe1—N392.17 (6)C8—C7—C6121.2 (2)
N1i—Fe1—N3i89.53 (6)C8—C7—H5119.4
N2—Fe1—N2i89.39 (7)H5—C7—C6119.4
N2—Fe1—N393.89 (7)C9—C8—C10117.0 (2)
N2—Fe1—N3i173.95 (6)C9—C8—C7118.3 (2)
N2i—Fe1—N3173.95 (6)C10—C8—C7124.7 (2)
N2i—Fe1—N3i93.89 (7)C11—C10—H6120.6
N3—Fe1—N3i83.30 (7)C11—C10—C8118.8 (2)
H13—O6—H13i131.0H6—C10—C8120.6
H13—O6—H14114.5C12—C11—H7119.8
H13i—O6—H14114.5C12—C11—C10120.4 (2)
C1—N1—Fe1130.1 (1)H7—C11—C10119.8
C1—N1—C5117.2 (2)H8—C12—N2118.5
C5—N1—Fe1112.6 (1)H8—C12—C11118.5
C9—N2—Fe1113.4 (1)C14—C13—N3122.3 (2)
C9—N2—C12116.6 (2)C14—C13—H9118.9
C12—N2—Fe1130.0 (1)H9—C13—N3118.9
C13—N3—Fe1130.2 (2)C15—C14—C13120.2 (3)
C13—N3—C17117.3 (2)C15—C14—H10119.9
C17—N3—Fe1112.5 (1)H10—C14—C13119.9
O4ii—N5—O4119.2 (6)C16—C15—C14119.8 (2)
O4ii—N5—O5120.4 (4)C16—C15—H11120.1
C2—C1—H1118.8H11—C15—C14120.1
C2—C1—N1122.3 (2)C17—C16—C15116.4 (2)
H1—C1—N1118.8C17—C16—C18118.5 (2)
C3—C2—C1120.4 (2)C18—C16—C15125.0 (2)
C3—C2—H2119.8C17i—C17—N3115.8 (2)
H2—C2—C1119.8C17i—C17—C16120.2 (2)
C4—C3—C2119.0 (2)C18i—C18—C16121.2 (2)
C4—C3—H3120.5C18i—C18—H12119.4
H3—C3—C2120.5H12—C18—C16119.4
C5—C4—C3117.2 (2)
N2—Fe1—N1—C1179.16 (18)N1—C5—C9—C8177.6 (2)
N1—Fe1—N2—C91.82 (13)C4—C5—C9—N2178.1 (2)
N1—Fe1—N3—C1389.81 (17)C4—C5—C9—C82.0 (3)
Fe1—N1—C1—C2176.4 (2)C4—C6—C7—C81.6 (4)
Fe1—N1—C5—C4176.7 (2)C6—C7—C8—C92.1 (3)
Fe1—N2—C9—C50.3 (2)C7—C8—C9—N2176.3 (2)
Fe1—N2—C9—C8179.8 (2)C7—C8—C9—C53.8 (3)
Fe1—N2—C12—C11175.9 (2)C7—C8—C10—C11177.5 (2)
Fe1—N3—C13—C14178.2 (2)C8—C10—C11—C120.0 (3)
Fe1—N3—C17—C16179.1 (2)C10—C11—C12—N23.2 (4)
N1—C1—C2—C30.6 (4)N3—C13—C14—C150.3 (3)
C1—C2—C3—C40.5 (4)C13—C14—C15—C160.4 (3)
C2—C3—C4—C50.2 (3)C14—C15—C16—C170.1 (3)
C3—C4—C5—N10.0 (2)C15—C16—C17—N30.8 (3)
C3—C4—C6—C7177.8 (2)C15—C16—C18—H121.6
N1—C5—C9—N22.3 (3)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H13···O1i0.872.022.657 (4)129
O6—H13···O2i0.872.383.053 (5)135
O6—H14···O4iii0.892.243.067 (8)154
Symmetry codes: (i) x, y, z+1/2; (iii) x1/2, y+1/2, z.
 

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