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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
CCDC reference: 258663
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (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
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·H2O | F(000) = 1546.00 |
Mr = 800.50 | Dx = 1.553 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: -c_2yc | Cell parameters from 12716 reflections |
a = 10.769 (8) Å | θ = 3.1–27.4° |
b = 24.58 (2) Å | µ = 0.52 mm−1 |
c = 13.274 (12) Å | T = 296 K |
β = 103.00 (3)° | Block, brown |
V = 3423 (5) Å3 | 0.20 × 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-1 | Rint = 0.024 |
ω scans | θmax = 27.4° |
Absorption correction: multi-scan (Higashi, 1995). | h = −12→13 |
Tmin = 0.732, Tmax = 0.904 | k = −31→31 |
16262 measured reflections | l = −17→17 |
3869 independent reflections | |
Refinement top
Refinement on F2 | H-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 = 1.02 | Δρmax = 0.71 e Å−3 |
3869 reflections | Δρmin = −0.49 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe1 | 0.0000 | 0.12256 (2) | 0.2500 | 0.0277 (1) | |
O1 | 0.1505 (3) | 0.4614 (1) | 0.1272 (2) | 0.1078 (9) | |
O2 | 0.1426 (3) | 0.3892 (1) | 0.2167 (2) | 0.124 (1) | |
O3 | 0.2222 (3) | 0.3865 (1) | 0.0849 (3) | 0.1078 (9) | |
O4 | 0.4204 (4) | 0.1109 (3) | 0.1971 (3) | 0.219 (3) | |
O5 | 0.5000 | 0.1821 (2) | 0.2500 | 0.172 (3) | |
O6 | 0.0000 | 0.4926 (2) | 0.2500 | 0.190 (3) | |
N1 | −0.1591 (1) | 0.12416 (6) | 0.1397 (1) | 0.0300 (3) | |
N2 | 0.0521 (1) | 0.17956 (7) | 0.1636 (1) | 0.0300 (3) | |
N3 | 0.0640 (1) | 0.06271 (7) | 0.1771 (1) | 0.0322 (4) | |
N4 | 0.1731 (3) | 0.4115 (1) | 0.1436 (2) | 0.0791 (8) | |
N5 | 0.5000 | 0.1343 (2) | 0.2500 | 0.0672 (9) | |
C1 | −0.2660 (2) | 0.09459 (9) | 0.1290 (2) | 0.0390 (5) | |
C2 | −0.3674 (2) | 0.0992 (1) | 0.0422 (2) | 0.0446 (5) | |
C3 | −0.3597 (2) | 0.1342 (1) | −0.0360 (2) | 0.0430 (5) | |
C4 | −0.2491 (2) | 0.16589 (9) | −0.0278 (2) | 0.0361 (4) | |
C5 | −0.1518 (2) | 0.15917 (8) | 0.0619 (1) | 0.0300 (4) | |
C6 | −0.2282 (2) | 0.2034 (1) | −0.1046 (2) | 0.0442 (5) | |
C7 | −0.1208 (2) | 0.2341 (1) | −0.0901 (2) | 0.0445 (5) | |
C8 | −0.0222 (2) | 0.22913 (8) | 0.0018 (2) | 0.0363 (4) | |
C9 | −0.0373 (2) | 0.19028 (8) | 0.0758 (1) | 0.0301 (4) | |
C10 | 0.0893 (2) | 0.26122 (9) | 0.0249 (2) | 0.0440 (5) | |
C11 | 0.1782 (2) | 0.2509 (1) | 0.1135 (2) | 0.0457 (5) | |
C12 | 0.1589 (2) | 0.20942 (9) | 0.1797 (2) | 0.0377 (5) | |
C13 | 0.1325 (2) | 0.0641 (1) | 0.1044 (2) | 0.0422 (5) | |
C14 | 0.1728 (2) | 0.0169 (1) | 0.0629 (2) | 0.0521 (6) | |
C15 | 0.1426 (2) | −0.0325 (1) | 0.0953 (2) | 0.0542 (6) | |
C16 | 0.0707 (2) | −0.03630 (9) | 0.1719 (2) | 0.0446 (5) | |
C17 | 0.0349 (2) | 0.01282 (8) | 0.2101 (2) | 0.0336 (4) | |
C18 | 0.0333 (3) | −0.0860 (1) | 0.2124 (2) | 0.0595 (7) | |
H1 | −0.2731 | 0.0702 | 0.1810 | 0.047* | |
H2 | −0.4403 | 0.0782 | 0.0379 | 0.053* | |
H3 | −0.4267 | 0.1371 | −0.0939 | 0.052* | |
H4 | −0.2896 | 0.2070 | −0.1659 | 0.053* | |
H5 | −0.1111 | 0.2587 | −0.1409 | 0.053* | |
H6 | 0.1020 | 0.2889 | −0.0195 | 0.053* | |
H7 | 0.2522 | 0.2716 | 0.1298 | 0.055* | |
H8 | 0.2231 | 0.2021 | 0.2378 | 0.045* | |
H9 | 0.1538 | 0.0977 | 0.0809 | 0.051* | |
H10 | 0.2205 | 0.0195 | 0.0128 | 0.063* | |
H11 | 0.1692 | −0.0639 | 0.0672 | 0.065* | |
H12 | 0.0550 | −0.1190 | 0.1866 | 0.071* | |
H13 | −0.0730 | 0.4780 | 0.2510 | 0.285* | 0.5 |
H14 | 0.0000 | 0.5290 | 0.2500 | 0.285* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0319 (2) | 0.0267 (2) | 0.0247 (2) | 0.0000 | 0.0069 (1) | 0.0000 |
O1 | 0.137 (2) | 0.080 (2) | 0.106 (2) | 0.008 (2) | 0.026 (2) | 0.015 (2) |
O2 | 0.118 (2) | 0.167 (3) | 0.082 (2) | −0.059 (2) | 0.010 (2) | 0.045 (2) |
O3 | 0.136 (3) | 0.084 (2) | 0.103 (2) | −0.027 (2) | 0.026 (2) | −0.006 (2) |
O4 | 0.141 (3) | 0.395 (7) | 0.139 (4) | −0.152 (4) | 0.070 (3) | −0.107 (4) |
O5 | 0.275 (7) | 0.085 (3) | 0.213 (6) | 0.0000 | 0.175 (6) | 0.0000 |
O6 | 0.175 (5) | 0.093 (4) | 0.337 (9) | 0.0000 | 0.132 (6) | 0.0000 |
N1 | 0.0331 (8) | 0.0293 (9) | 0.0282 (8) | −0.0004 (6) | 0.0081 (6) | −0.0026 (7) |
N2 | 0.0334 (8) | 0.0287 (9) | 0.0283 (8) | −0.0011 (6) | 0.0078 (7) | −0.0016 (7) |
N3 | 0.0357 (9) | 0.032 (1) | 0.0287 (9) | 0.0008 (7) | 0.0062 (7) | −0.0013 (7) |
N4 | 0.066 (2) | 0.097 (2) | 0.065 (2) | −0.030 (2) | −0.005 (1) | 0.013 (2) |
N5 | 0.061 (2) | 0.079 (3) | 0.071 (2) | 0.0000 | 0.035 (2) | 0.0000 |
C1 | 0.038 (1) | 0.043 (1) | 0.037 (1) | −0.0060 (9) | 0.0084 (9) | −0.000 (1) |
C2 | 0.035 (1) | 0.053 (1) | 0.044 (1) | −0.0083 (9) | 0.0049 (9) | −0.005 (1) |
C3 | 0.037 (1) | 0.049 (1) | 0.038 (1) | 0.0032 (9) | −0.0009 (9) | −0.008 (1) |
C4 | 0.042 (1) | 0.035 (1) | 0.030 (1) | 0.0072 (8) | 0.0048 (8) | −0.0037 (9) |
C5 | 0.0351 (9) | 0.028 (1) | 0.028 (1) | 0.0043 (7) | 0.0081 (8) | −0.0030 (8) |
C6 | 0.055 (1) | 0.043 (1) | 0.030 (1) | 0.010 (1) | 0.0001 (9) | 0.004 (1) |
C7 | 0.057 (1) | 0.041 (1) | 0.036 (1) | 0.009 (1) | 0.011 (1) | 0.010 (1) |
C8 | 0.046 (1) | 0.031 (1) | 0.034 (1) | 0.0046 (9) | 0.0150 (9) | 0.0031 (9) |
C9 | 0.037 (1) | 0.026 (1) | 0.029 (1) | 0.0032 (7) | 0.0102 (8) | −0.0009 (8) |
C10 | 0.054 (1) | 0.036 (1) | 0.047 (1) | −0.001 (1) | 0.022 (1) | 0.008 (1) |
C11 | 0.047 (1) | 0.045 (1) | 0.048 (1) | −0.012 (1) | 0.016 (1) | 0.000 (1) |
C12 | 0.039 (1) | 0.038 (1) | 0.036 (1) | −0.0069 (9) | 0.0079 (9) | −0.0008 (9) |
C13 | 0.048 (1) | 0.047 (1) | 0.035 (1) | 0.002 (1) | 0.0158 (9) | −0.005 (1) |
C14 | 0.055 (1) | 0.057 (2) | 0.049 (1) | 0.006 (1) | 0.022 (1) | −0.011 (1) |
C15 | 0.059 (1) | 0.046 (1) | 0.060 (2) | 0.011 (1) | 0.017 (1) | −0.017 (1) |
C16 | 0.044 (1) | 0.034 (1) | 0.052 (1) | 0.0049 (9) | 0.003 (1) | −0.007 (1) |
C17 | 0.034 (1) | 0.031 (1) | 0.034 (1) | 0.0001 (8) | 0.0029 (8) | −0.0030 (9) |
C18 | 0.064 (2) | 0.032 (1) | 0.082 (2) | 0.004 (1) | 0.014 (1) | −0.007 (1) |
Geometric parameters (Å, º) top
Fe1—N1 | 1.988 (1) | C3—H3 | 0.93 |
Fe1—N1i | 1.988 (1) | C4—C5 | 1.408 (2) |
Fe1—N2 | 1.971 (2) | C4—C6 | 1.430 (3) |
Fe1—N2i | 1.971 (2) | C5—C9 | 1.427 (3) |
Fe1—N3 | 1.968 (2) | C6—C7 | 1.357 (3) |
Fe1—N3i | 1.968 (2) | C6—H4 | 0.93 |
O1—N4 | 1.259 (5) | C7—C8 | 1.431 (3) |
O2—N4 | 1.222 (5) | C7—H5 | 0.93 |
O3—N4 | 1.204 (5) | C8—C9 | 1.406 (3) |
O4—N5 | 1.134 (5) | C8—C10 | 1.412 (3) |
O5—N5 | 1.174 (7) | C10—C11 | 1.363 (3) |
O6—H13 | 0.87 | C10—H6 | 0.93 |
O6—H13i | 0.87 | C11—C12 | 1.391 (3) |
O6—H14 | 0.89 | C11—H7 | 0.93 |
N1—C1 | 1.341 (3) | C12—H8 | 0.93 |
N1—C5 | 1.361 (3) | C13—C14 | 1.394 (4) |
N2—C9 | 1.360 (2) | C13—H9 | 0.93 |
N2—C12 | 1.341 (3) | C14—C15 | 1.353 (4) |
N3—C13 | 1.340 (3) | C14—H10 | 0.93 |
N3—C17 | 1.362 (3) | C15—C16 | 1.414 (4) |
N5—O4ii | 1.134 (5) | C15—H11 | 0.93 |
C1—C2 | 1.403 (3) | C16—C17 | 1.397 (3) |
C1—H1 | 0.93 | C16—C18 | 1.428 (4) |
C2—C3 | 1.366 (3) | C17—C17i | 1.430 (3) |
C2—H2 | 0.93 | C18—C18i | 1.353 (5) |
C3—C4 | 1.406 (3) | C18—H12 | 0.93 |
| | | |
N1—Fe1—N1i | 177.73 (7) | C5—C4—C6 | 118.2 (2) |
N1—Fe1—N2 | 82.43 (6) | C6—C4—C3 | 124.6 (2) |
N1—Fe1—N2i | 95.95 (6) | C9—C5—N1 | 115.9 (1) |
N1—Fe1—N3 | 89.53 (6) | C9—C5—C4 | 120.2 (2) |
N1—Fe1—N3i | 92.17 (6) | C7—C6—C4 | 121.5 (2) |
N1i—Fe1—N2 | 95.95 (6) | C7—C6—H4 | 119.2 |
N1i—Fe1—N2i | 82.43 (6) | H4—C6—C4 | 119.2 |
N1i—Fe1—N3 | 92.17 (6) | C8—C7—C6 | 121.2 (2) |
N1i—Fe1—N3i | 89.53 (6) | C8—C7—H5 | 119.4 |
N2—Fe1—N2i | 89.39 (7) | H5—C7—C6 | 119.4 |
N2—Fe1—N3 | 93.89 (7) | C9—C8—C10 | 117.0 (2) |
N2—Fe1—N3i | 173.95 (6) | C9—C8—C7 | 118.3 (2) |
N2i—Fe1—N3 | 173.95 (6) | C10—C8—C7 | 124.7 (2) |
N2i—Fe1—N3i | 93.89 (7) | C11—C10—H6 | 120.6 |
N3—Fe1—N3i | 83.30 (7) | C11—C10—C8 | 118.8 (2) |
H13—O6—H13i | 131.0 | H6—C10—C8 | 120.6 |
H13—O6—H14 | 114.5 | C12—C11—H7 | 119.8 |
H13i—O6—H14 | 114.5 | C12—C11—C10 | 120.4 (2) |
C1—N1—Fe1 | 130.1 (1) | H7—C11—C10 | 119.8 |
C1—N1—C5 | 117.2 (2) | H8—C12—N2 | 118.5 |
C5—N1—Fe1 | 112.6 (1) | H8—C12—C11 | 118.5 |
C9—N2—Fe1 | 113.4 (1) | C14—C13—N3 | 122.3 (2) |
C9—N2—C12 | 116.6 (2) | C14—C13—H9 | 118.9 |
C12—N2—Fe1 | 130.0 (1) | H9—C13—N3 | 118.9 |
C13—N3—Fe1 | 130.2 (2) | C15—C14—C13 | 120.2 (3) |
C13—N3—C17 | 117.3 (2) | C15—C14—H10 | 119.9 |
C17—N3—Fe1 | 112.5 (1) | H10—C14—C13 | 119.9 |
O4ii—N5—O4 | 119.2 (6) | C16—C15—C14 | 119.8 (2) |
O4ii—N5—O5 | 120.4 (4) | C16—C15—H11 | 120.1 |
C2—C1—H1 | 118.8 | H11—C15—C14 | 120.1 |
C2—C1—N1 | 122.3 (2) | C17—C16—C15 | 116.4 (2) |
H1—C1—N1 | 118.8 | C17—C16—C18 | 118.5 (2) |
C3—C2—C1 | 120.4 (2) | C18—C16—C15 | 125.0 (2) |
C3—C2—H2 | 119.8 | C17i—C17—N3 | 115.8 (2) |
H2—C2—C1 | 119.8 | C17i—C17—C16 | 120.2 (2) |
C4—C3—C2 | 119.0 (2) | C18i—C18—C16 | 121.2 (2) |
C4—C3—H3 | 120.5 | C18i—C18—H12 | 119.4 |
H3—C3—C2 | 120.5 | H12—C18—C16 | 119.4 |
C5—C4—C3 | 117.2 (2) | | |
| | | |
N2—Fe1—N1—C1 | 179.16 (18) | N1—C5—C9—C8 | −177.6 (2) |
N1—Fe1—N2—C9 | −1.82 (13) | C4—C5—C9—N2 | −178.1 (2) |
N1—Fe1—N3—C13 | 89.81 (17) | C4—C5—C9—C8 | 2.0 (3) |
Fe1—N1—C1—C2 | −176.4 (2) | C4—C6—C7—C8 | 1.6 (4) |
Fe1—N1—C5—C4 | 176.7 (2) | C6—C7—C8—C9 | 2.1 (3) |
Fe1—N2—C9—C5 | 0.3 (2) | C7—C8—C9—N2 | 176.3 (2) |
Fe1—N2—C9—C8 | −179.8 (2) | C7—C8—C9—C5 | −3.8 (3) |
Fe1—N2—C12—C11 | −175.9 (2) | C7—C8—C10—C11 | −177.5 (2) |
Fe1—N3—C13—C14 | 178.2 (2) | C8—C10—C11—C12 | −0.0 (3) |
Fe1—N3—C17—C16 | −179.1 (2) | C10—C11—C12—N2 | −3.2 (4) |
N1—C1—C2—C3 | 0.6 (4) | N3—C13—C14—C15 | 0.3 (3) |
C1—C2—C3—C4 | −0.5 (4) | C13—C14—C15—C16 | −0.4 (3) |
C2—C3—C4—C5 | 0.2 (3) | C14—C15—C16—C17 | −0.1 (3) |
C3—C4—C5—N1 | 0.0 (2) | C15—C16—C17—N3 | 0.8 (3) |
C3—C4—C6—C7 | 177.8 (2) | C15—C16—C18—H12 | −1.6 |
N1—C5—C9—N2 | 2.3 (3) | | |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x+1, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H13···O1i | 0.87 | 2.02 | 2.657 (4) | 129 |
O6—H13···O2i | 0.87 | 2.38 | 3.053 (5) | 135 |
O6—H14···O4iii | 0.89 | 2.24 | 3.067 (8) | 154 |
Symmetry codes: (i) −x, y, −z+1/2; (iii) x−1/2, y+1/2, z. |
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