Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807045060/ww2093sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807045060/ww2093Isup2.hkl |
CCDC reference: 663632
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (N-C) = 0.003 Å
- R factor = 0.037
- wR factor = 0.113
- Data-to-parameter ratio = 12.8
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - N1 .. 5.57 su PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.17 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.47 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4 O11 -FE1 -N1 -C3 -146.90 1.10 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 10 O11 -FE1 -N1 -C1 24.50 1.30 1.555 1.555 1.555 1.555 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT731_ALERT_1_C Bond Calc 0.84(2), Rep 0.841(9) ...... 2.22 su-Ra O7 -H7A 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(2), Rep 0.841(9) ...... 2.22 su-Ra O10 -H10B 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(2), Rep 0.838(9) ...... 2.22 su-Ra O1W -H1WB 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(2), Rep 0.841(9) ...... 2.22 su-Ra O7 -H7A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(2), Rep 0.841(9) ...... 2.22 su-Ra O10 -H10B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(2), Rep 0.838(9) ...... 2.22 su-Ra O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(2), Rep 0.838(9) ...... 2.22 su-Ra O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(2), Rep 0.838(9) ...... 2.22 su-Ra O1W -H1# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.95(3), Rep 1.946(14) ...... 2.14 su-Ra H9B -O1W 1.555 1.445 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Fe1 (2) 1.73 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 25
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 4 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For general background, see: Cai et al. (2001). For related structures, see: Cai et al. (2003). For related literature, see: Cai, et al. (2005).
A solution of FeCl2 (200 mg, 1.00 mmol) in CH3OH (20 ml) was slowly added to a solution of 1,3,5-triazinane-2,4,6-trione (260 mg, 1.95 mmol) in CH3OH (10 ml). The resultant pale green solution was stirred under N2 for 2 h at 323 K and then filtered. After addition of diethyl ether (20 ml), the filtrate was cooled to 253 K. Microcrystalline material was collected after 24 h and dried under vacuum (yield: 237 mg, 53%). Green blocks suitable for X-ray diffraction were obtained in 2 d by slow diffusion of diethyl ether into a dilute solution of the title complex in methanol. The assigned structure was substantiated by elemental analysis; calculated for C6H18N6FeO13: C 16.47, H 4.12, N 19.21%; found: C 16.43, H 4.18, N 19.17%.
The structure was solved using direct methods followed by Fourier synthesis. Non-H atoms were refined anisotropically. The water/nitrogen H atoms were located and isotropically refined, with the O—H/N—H and H···H for water molecules distances restrained to 0.84 (1) and 1.37 (2) Å, respectively. All other H atoms were placed in calculated positions (C—H = 0.93 or 0.97 Å), and were included in the refinement using the riding-model approximation. Uiso values were set equal to 1.5Ueq(parent atom) for water/nitrogen H atoms and to 1.2Ueq(parent atom) for all other H atoms.
Recently we reported a series of one-dimensional helical Ag(I) compounds containing 8-hydroxyquinoline coordinating groups (Cai et al., 2001 and 2003). As a part of the structural studies of the compounds involving the oxygen-nitrogen chelating ligand (Cai et al., 2005), here we report the synthesis and structure of the compound, pentaaqua(1,3,5-triazinanyl-2,4,6-trione)iron(II) 1,3,5-triazinanate-2,4,6-trione dihydrate, namely [Fe(C3H2N3O3)(H2O)5]+(C3H2N3O3)- 2H2O (Scheme 1).
Fig.1 shows that the molecule of [Fe(C3H2N3O3)(H2O)5]+(C3H2N3O3)- 2H2O consists of one cation [Fe(C3H2N3O3)(H2O)5]+, one anion (C3H2N3O3)- and two water molecules. The FeII atom exhibits a FeNO5 octahedral coordination geometry arising from one N-bonded 1,3,5-triazinanyl-2,4,6-trione molecule and five O atoms of water molecules. The uncoordinated 1,3,5-triazinanyl-2,4,6-trione anion and uncoordinated water molecules interact with the cation through O—H···O, O—H···N and N—H···O hydrogen bonds (Table 1), generating a three-dimensional network.
For general background, see: Cai et al. (2001). For related structures, see: Cai et al. (2003). For related literature, see: Cai, et al. (2005).
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).
Fig. 1. The structure of title molecule, with its atom-numbering scheme, is shown at the 50% probability level. |
[Fe(C3H2N3O3)(H2O)5](C3H2N3O3)·2H2O | F(000) = 904 |
Mr = 438.11 | Dx = 1.809 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 4778 reflections |
a = 14.0563 (2) Å | θ = 2.4–27.4° |
b = 6.6947 (1) Å | µ = 1.02 mm−1 |
c = 17.2336 (3) Å | T = 298 K |
β = 97.408 (1)° | Block, green |
V = 1608.19 (4) Å3 | 0.20 × 0.17 × 0.15 mm |
Z = 4 |
Bruker SMART CCD area-detector diffractometer | 3691 independent reflections |
Radiation source: fine-focus sealed tube | 3064 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 27.5°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→17 |
Tmin = 0.822, Tmax = 0.862 | k = −8→6 |
14409 measured reflections | l = −22→22 |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.113 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.062P)2 + 0.9167P] where P = (Fo2 + 2Fc2)/3 |
3691 reflections | (Δ/σ)max < 0.001 |
289 parameters | Δρmax = 0.36 e Å−3 |
25 restraints | Δρmin = −0.45 e Å−3 |
[Fe(C3H2N3O3)(H2O)5](C3H2N3O3)·2H2O | V = 1608.19 (4) Å3 |
Mr = 438.11 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 14.0563 (2) Å | µ = 1.02 mm−1 |
b = 6.6947 (1) Å | T = 298 K |
c = 17.2336 (3) Å | 0.20 × 0.17 × 0.15 mm |
β = 97.408 (1)° |
Bruker SMART CCD area-detector diffractometer | 3691 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3064 reflections with I > 2σ(I) |
Tmin = 0.822, Tmax = 0.862 | Rint = 0.028 |
14409 measured reflections |
R[F2 > 2σ(F2)] = 0.037 | 25 restraints |
wR(F2) = 0.113 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | Δρmax = 0.36 e Å−3 |
3691 reflections | Δρmin = −0.45 e Å−3 |
289 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Fe1 | −0.05822 (2) | 0.17964 (5) | 0.678490 (17) | 0.02687 (13) | |
O1 | −0.01859 (11) | 0.1853 (3) | 0.87539 (9) | 0.0296 (4) | |
O2 | 0.30290 (12) | 0.2819 (3) | 0.93035 (10) | 0.0421 (5) | |
O3 | 0.17061 (11) | 0.1783 (3) | 0.68074 (9) | 0.0327 (4) | |
O4 | 0.41363 (11) | 0.1655 (3) | 0.75242 (8) | 0.0289 (4) | |
O5 | 0.60977 (11) | 0.2088 (3) | 0.56299 (10) | 0.0377 (4) | |
O6 | 0.28965 (12) | 0.2944 (3) | 0.50276 (10) | 0.0433 (5) | |
O7 | −0.00205 (11) | 0.4449 (3) | 0.62062 (9) | 0.0302 (4) | |
H7B | 0.0276 (17) | 0.510 (3) | 0.6578 (11) | 0.045* | |
H7A | −0.0367 (17) | 0.512 (3) | 0.5867 (11) | 0.045* | |
O8 | 0.00260 (12) | −0.0127 (3) | 0.59652 (10) | 0.0372 (4) | |
H8A | 0.0619 (7) | −0.014 (4) | 0.6028 (18) | 0.056* | |
H8B | −0.0266 (16) | −0.107 (3) | 0.5730 (18) | 0.056* | |
O9 | −0.13082 (12) | −0.0603 (3) | 0.72935 (10) | 0.0329 (4) | |
H9B | −0.1713 (16) | −0.122 (4) | 0.6988 (13) | 0.049* | |
H9A | −0.0971 (17) | −0.129 (3) | 0.7635 (13) | 0.049* | |
O10 | −0.13586 (11) | 0.3992 (3) | 0.74129 (9) | 0.0284 (3) | |
H10A | −0.0988 (15) | 0.472 (3) | 0.7713 (13) | 0.043* | |
H10B | −0.1783 (14) | 0.459 (3) | 0.7112 (13) | 0.043* | |
O11 | −0.18778 (12) | 0.1871 (3) | 0.59092 (10) | 0.0404 (5) | |
H11A | −0.2439 (11) | 0.197 (5) | 0.6014 (16) | 0.061* | |
H11B | −0.179 (2) | 0.201 (5) | 0.5442 (8) | 0.061* | |
O1W | 0.74356 (12) | 0.6644 (3) | 0.65640 (9) | 0.0329 (4) | |
H1WB | 0.6986 (14) | 0.692 (5) | 0.6821 (12) | 0.049* | |
H1WA | 0.7299 (18) | 0.657 (5) | 0.6077 (6) | 0.049* | |
O2W | 0.09420 (12) | 0.3139 (3) | 0.49336 (10) | 0.0339 (4) | |
H2WA | 0.1543 (8) | 0.301 (5) | 0.4958 (15) | 0.051* | |
H2WB | 0.0736 (17) | 0.326 (5) | 0.5373 (10) | 0.051* | |
N1 | 0.06881 (12) | 0.1824 (3) | 0.77285 (10) | 0.0205 (4) | |
N2 | 0.14088 (12) | 0.2369 (3) | 0.90343 (10) | 0.0247 (4) | |
H2 | 0.1357 (19) | 0.244 (4) | 0.9520 (7) | 0.030* | |
N3 | 0.23620 (13) | 0.2187 (3) | 0.80582 (11) | 0.0286 (4) | |
H3 | 0.2910 (11) | 0.217 (4) | 0.7898 (16) | 0.034* | |
N4 | 0.35144 (13) | 0.2299 (3) | 0.62800 (10) | 0.0246 (4) | |
H4 | 0.2955 (10) | 0.223 (4) | 0.6421 (15) | 0.029* | |
N5 | 0.51845 (12) | 0.1830 (3) | 0.66238 (10) | 0.0232 (4) | |
N6 | 0.45021 (13) | 0.2501 (3) | 0.53267 (10) | 0.0274 (4) | |
H6 | 0.4638 (19) | 0.262 (4) | 0.4856 (8) | 0.033* | |
C1 | 0.05928 (15) | 0.2003 (3) | 0.85001 (12) | 0.0207 (4) | |
C2 | 0.23144 (15) | 0.2485 (4) | 0.88340 (12) | 0.0264 (5) | |
C3 | 0.15702 (15) | 0.1924 (3) | 0.75000 (12) | 0.0220 (4) | |
C4 | 0.42988 (14) | 0.1913 (3) | 0.68387 (12) | 0.0213 (4) | |
C5 | 0.53042 (15) | 0.2133 (3) | 0.58650 (12) | 0.0242 (4) | |
C6 | 0.35972 (15) | 0.2595 (4) | 0.55118 (12) | 0.0256 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.02585 (19) | 0.0331 (2) | 0.02092 (18) | −0.00181 (13) | 0.00026 (12) | −0.00010 (12) |
O1 | 0.0202 (7) | 0.0491 (10) | 0.0200 (7) | −0.0022 (7) | 0.0045 (6) | 0.0003 (7) |
O2 | 0.0236 (8) | 0.0810 (14) | 0.0206 (8) | −0.0096 (9) | −0.0013 (6) | −0.0031 (8) |
O3 | 0.0228 (8) | 0.0586 (12) | 0.0171 (7) | −0.0006 (7) | 0.0034 (6) | −0.0039 (7) |
O4 | 0.0259 (8) | 0.0444 (10) | 0.0171 (7) | 0.0045 (7) | 0.0052 (6) | 0.0065 (6) |
O5 | 0.0188 (8) | 0.0717 (13) | 0.0231 (8) | 0.0025 (8) | 0.0048 (6) | 0.0027 (8) |
O6 | 0.0200 (8) | 0.0872 (16) | 0.0216 (8) | 0.0053 (8) | −0.0016 (6) | 0.0065 (9) |
O7 | 0.0311 (8) | 0.0352 (9) | 0.0231 (8) | −0.0038 (7) | −0.0002 (6) | 0.0045 (7) |
O8 | 0.0258 (8) | 0.0480 (11) | 0.0378 (9) | −0.0018 (8) | 0.0038 (7) | −0.0163 (8) |
O9 | 0.0293 (8) | 0.0351 (9) | 0.0322 (9) | −0.0057 (7) | −0.0047 (7) | 0.0081 (7) |
O10 | 0.0248 (8) | 0.0321 (9) | 0.0267 (8) | 0.0017 (7) | −0.0021 (6) | −0.0028 (7) |
O11 | 0.0227 (8) | 0.0769 (14) | 0.0206 (8) | 0.0017 (9) | −0.0007 (6) | 0.0016 (8) |
O1W | 0.0266 (8) | 0.0496 (11) | 0.0224 (8) | 0.0031 (7) | 0.0031 (6) | −0.0009 (7) |
O2W | 0.0244 (8) | 0.0484 (11) | 0.0289 (8) | 0.0003 (8) | 0.0034 (6) | −0.0008 (7) |
N1 | 0.0170 (8) | 0.0287 (9) | 0.0156 (8) | −0.0003 (7) | 0.0019 (6) | −0.0002 (7) |
N2 | 0.0206 (9) | 0.0389 (11) | 0.0146 (8) | −0.0012 (8) | 0.0026 (7) | −0.0025 (8) |
N3 | 0.0160 (8) | 0.0514 (13) | 0.0187 (9) | −0.0008 (8) | 0.0031 (7) | −0.0031 (8) |
N4 | 0.0160 (8) | 0.0397 (11) | 0.0186 (8) | 0.0010 (8) | 0.0042 (7) | 0.0019 (8) |
N5 | 0.0192 (8) | 0.0322 (10) | 0.0180 (8) | 0.0016 (7) | 0.0018 (6) | 0.0010 (7) |
N6 | 0.0204 (9) | 0.0475 (12) | 0.0146 (8) | 0.0008 (8) | 0.0029 (7) | 0.0006 (8) |
C1 | 0.0199 (9) | 0.0238 (11) | 0.0182 (9) | 0.0004 (8) | 0.0015 (7) | 0.0007 (8) |
C2 | 0.0236 (10) | 0.0370 (12) | 0.0183 (10) | −0.0012 (9) | 0.0012 (8) | 0.0009 (9) |
C3 | 0.0207 (10) | 0.0275 (11) | 0.0175 (9) | 0.0004 (8) | 0.0010 (7) | −0.0008 (8) |
C4 | 0.0198 (10) | 0.0242 (11) | 0.0199 (10) | 0.0007 (8) | 0.0021 (8) | −0.0005 (8) |
C5 | 0.0187 (9) | 0.0338 (12) | 0.0198 (10) | 0.0002 (8) | 0.0022 (8) | 0.0001 (8) |
C6 | 0.0191 (9) | 0.0386 (12) | 0.0189 (10) | 0.0008 (9) | 0.0015 (8) | −0.0010 (9) |
Fe1—O9 | 2.1495 (17) | O1W—H1WA | 0.837 (10) |
Fe1—O8 | 2.1671 (17) | O2W—H2WA | 0.844 (10) |
Fe1—O10 | 2.1973 (16) | O2W—H2WB | 0.849 (10) |
Fe1—O11 | 2.2109 (16) | N1—C3 | 1.350 (3) |
Fe1—O7 | 2.2303 (17) | N1—C1 | 1.359 (3) |
Fe1—N1 | 2.2549 (16) | N2—C2 | 1.363 (3) |
O1—C1 | 1.234 (3) | N2—C1 | 1.397 (3) |
O2—C2 | 1.226 (3) | N2—H2 | 0.851 (10) |
O3—C3 | 1.237 (3) | N3—C2 | 1.362 (3) |
O4—C4 | 1.244 (2) | N3—C3 | 1.385 (3) |
O5—C5 | 1.235 (3) | N3—H3 | 0.851 (10) |
O6—C6 | 1.228 (3) | N4—C6 | 1.358 (3) |
O7—H7B | 0.839 (10) | N4—C4 | 1.391 (3) |
O7—H7A | 0.841 (9) | N4—H4 | 0.853 (10) |
O8—H8A | 0.827 (9) | N5—C4 | 1.345 (3) |
O8—H8B | 0.829 (10) | N5—C5 | 1.355 (3) |
O9—H9B | 0.833 (10) | N6—C6 | 1.352 (3) |
O9—H9A | 0.843 (10) | N6—C5 | 1.387 (3) |
O10—H10A | 0.842 (10) | N6—H6 | 0.860 (10) |
O10—H10B | 0.841 (9) | C3—O3 | 1.237 (3) |
O11—H11A | 0.835 (10) | C4—O4 | 1.244 (2) |
O11—H11B | 0.835 (10) | C6—O6 | 1.228 (3) |
O1W—H1WB | 0.838 (9) | ||
O9—Fe1—O8 | 93.99 (8) | C1—N1—Fe1 | 122.52 (14) |
O9—Fe1—O10 | 90.40 (7) | C2—N2—C1 | 123.87 (18) |
O8—Fe1—O10 | 168.93 (6) | C2—N2—H2 | 116.6 (18) |
O9—Fe1—O11 | 84.41 (7) | C1—N2—H2 | 119.4 (18) |
O8—Fe1—O11 | 85.87 (7) | C2—N3—C3 | 124.30 (19) |
O10—Fe1—O11 | 84.46 (7) | C2—N3—H3 | 118.8 (19) |
O9—Fe1—O7 | 172.46 (6) | C3—N3—H3 | 116.9 (19) |
O8—Fe1—O7 | 89.41 (7) | C6—N4—C4 | 122.80 (19) |
O10—Fe1—O7 | 85.09 (7) | C6—N4—H4 | 118.9 (18) |
O11—Fe1—O7 | 89.12 (7) | C4—N4—H4 | 118.0 (18) |
O9—Fe1—O7 | 172.46 (6) | C4—N5—C5 | 119.60 (18) |
O8—Fe1—O7 | 89.41 (7) | C6—N6—C5 | 123.98 (18) |
O10—Fe1—O7 | 85.09 (7) | C6—N6—H6 | 123.2 (19) |
O11—Fe1—O7 | 89.12 (7) | C5—N6—H6 | 112.8 (19) |
O9—Fe1—N1 | 94.91 (6) | O1—C1—N1 | 122.93 (19) |
O8—Fe1—N1 | 97.63 (6) | O1—C1—N2 | 118.11 (19) |
O10—Fe1—N1 | 92.10 (6) | N1—C1—N2 | 118.96 (18) |
O11—Fe1—N1 | 176.48 (7) | O2—C2—N3 | 122.3 (2) |
O7—Fe1—N1 | 91.31 (6) | O2—C2—N2 | 123.7 (2) |
O7—Fe1—N1 | 91.31 (6) | N3—C2—N2 | 113.95 (18) |
Fe1—O7—H7B | 103.8 (18) | O3—C3—N1 | 122.67 (18) |
Fe1—O7—H7A | 122.0 (19) | O3—C3—N1 | 122.67 (18) |
H7B—O7—H7A | 116.2 (14) | O3—C3—N3 | 118.01 (19) |
Fe1—O8—H8A | 113.3 (19) | O3—C3—N3 | 118.01 (19) |
Fe1—O8—H8B | 124 (2) | N1—C3—N3 | 119.32 (18) |
H8A—O8—H8B | 119.0 (15) | O4—C4—N5 | 123.06 (18) |
Fe1—O9—H9B | 115.7 (19) | O4—C4—N5 | 123.06 (18) |
Fe1—O9—H9A | 116.1 (19) | O4—C4—N4 | 117.18 (19) |
H9B—O9—H9A | 116.6 (14) | O4—C4—N4 | 117.18 (19) |
Fe1—O10—H10A | 112.6 (18) | N5—C4—N4 | 119.76 (18) |
Fe1—O10—H10B | 112.0 (18) | O5—C5—N5 | 122.86 (19) |
H10A—O10—H10B | 115.8 (14) | O5—C5—N6 | 118.40 (19) |
Fe1—O11—H11A | 125 (2) | N5—C5—N6 | 118.74 (19) |
Fe1—O11—H11B | 117 (2) | O6—C6—N6 | 123.0 (2) |
H11A—O11—H11B | 117.4 (15) | O6—C6—N6 | 123.0 (2) |
H1WB—O1W—H1WA | 116.8 (14) | O6—C6—N4 | 121.9 (2) |
H2WA—O2W—H2WB | 114.9 (14) | O6—C6—N4 | 121.9 (2) |
C3—N1—C1 | 119.42 (17) | N6—C6—N4 | 115.12 (19) |
C3—N1—Fe1 | 117.50 (13) | ||
O9—Fe1—N1—C3 | 134.41 (15) | C1—N1—C3—O3 | −179.6 (2) |
O8—Fe1—N1—C3 | 39.71 (16) | Fe1—N1—C3—O3 | −8.0 (3) |
O10—Fe1—N1—C3 | −135.00 (15) | C1—N1—C3—N3 | 0.6 (3) |
O11—Fe1—N1—C3 | −146.9 (11) | Fe1—N1—C3—N3 | 172.28 (16) |
O7—Fe1—N1—C3 | −49.86 (15) | C2—N3—C3—O3 | 175.8 (2) |
O7—Fe1—N1—C3 | −49.86 (15) | C2—N3—C3—O3 | 175.8 (2) |
O9—Fe1—N1—C1 | −54.23 (17) | C2—N3—C3—N1 | −4.4 (3) |
O8—Fe1—N1—C1 | −148.93 (16) | C5—N5—C4—O4 | −179.8 (2) |
O10—Fe1—N1—C1 | 36.36 (16) | C5—N5—C4—O4 | −179.8 (2) |
O11—Fe1—N1—C1 | 24.5 (13) | C5—N5—C4—N4 | 0.3 (3) |
O7—Fe1—N1—C1 | 121.50 (16) | C6—N4—C4—O4 | −179.6 (2) |
O7—Fe1—N1—C1 | 121.50 (16) | C6—N4—C4—O4 | −179.6 (2) |
C3—N1—C1—O1 | −177.2 (2) | C6—N4—C4—N5 | 0.3 (3) |
Fe1—N1—C1—O1 | 11.6 (3) | C4—N5—C5—O5 | 179.6 (2) |
C3—N1—C1—N2 | 2.6 (3) | C4—N5—C5—N6 | −0.8 (3) |
Fe1—N1—C1—N2 | −168.57 (15) | C6—N6—C5—O5 | −179.7 (2) |
C2—N2—C1—O1 | 177.2 (2) | C6—N6—C5—N5 | 0.6 (4) |
C2—N2—C1—N1 | −2.7 (3) | C5—N6—C6—O6 | 179.2 (2) |
C3—N3—C2—O2 | −176.0 (2) | C5—N6—C6—O6 | 179.2 (2) |
C3—N3—C2—N2 | 4.3 (4) | C5—N6—C6—N4 | −0.1 (4) |
C1—N2—C2—O2 | 179.5 (2) | C4—N4—C6—O6 | −179.7 (2) |
C1—N2—C2—N3 | −0.7 (3) | C4—N4—C6—O6 | −179.7 (2) |
C1—N1—C3—O3 | −179.6 (2) | C4—N4—C6—N6 | −0.4 (3) |
Fe1—N1—C3—O3 | −8.0 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7B···O4i | 0.84 (1) | 1.96 (1) | 2.795 (2) | 175 (3) |
O7—H7A···O2Wii | 0.84 (1) | 1.91 (1) | 2.736 (2) | 170 (3) |
O8—H8A···O3 | 0.83 (1) | 2.29 (2) | 2.904 (2) | 131 (2) |
O8—H8A···O2iii | 0.83 (1) | 2.47 (2) | 3.147 (2) | 140 (2) |
O8—H8B···O2Wiv | 0.83 (1) | 1.96 (1) | 2.788 (2) | 174 (3) |
O9—H9B···O1Wv | 0.83 (1) | 1.95 (1) | 2.743 (2) | 160 (2) |
O9—H9A···N5iii | 0.84 (1) | 2.02 (1) | 2.858 (2) | 174 (3) |
O10—H10A···N5i | 0.84 (1) | 2.06 (1) | 2.895 (2) | 172 (2) |
O10—H10B···O1Wvi | 0.84 (1) | 1.93 (1) | 2.743 (2) | 163 (2) |
O11—H11A···O5vi | 0.84 (1) | 2.08 (2) | 2.828 (2) | 149 (3) |
O11—H11B···O2vii | 0.84 (1) | 1.95 (1) | 2.761 (2) | 164 (3) |
O1W—H1WB···O10i | 0.84 (1) | 2.18 (2) | 2.926 (2) | 148 (3) |
O1W—H1WB···O9i | 0.84 (1) | 2.54 (3) | 3.075 (3) | 123 (3) |
O1W—H1WB···O1i | 0.84 (1) | 2.60 (2) | 3.142 (2) | 124 (2) |
O1W—H1WA···O6viii | 0.84 (1) | 1.92 (1) | 2.736 (2) | 166 (3) |
O2W—H2WA···O6 | 0.84 (1) | 1.89 (1) | 2.734 (2) | 176 (3) |
O2W—H2WB···O7 | 0.85 (1) | 2.05 (1) | 2.859 (2) | 158 (3) |
N3—H3···O4 | 0.85 (1) | 1.95 (1) | 2.790 (2) | 170 (3) |
N4—H4···O3 | 0.85 (1) | 1.98 (1) | 2.829 (2) | 174 (3) |
N6—H6···O1ix | 0.86 (1) | 1.98 (1) | 2.834 (2) | 173 (3) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+3/2; (ii) −x, −y+1, −z+1; (iii) −x+1/2, y−1/2, −z+3/2; (iv) −x, −y, −z+1; (v) x−1, y−1, z; (vi) x−1, y, z; (vii) x−1/2, −y+1/2, z−1/2; (viii) −x+1, −y+1, −z+1; (ix) x+1/2, −y+1/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Fe(C3H2N3O3)(H2O)5](C3H2N3O3)·2H2O |
Mr | 438.11 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 298 |
a, b, c (Å) | 14.0563 (2), 6.6947 (1), 17.2336 (3) |
β (°) | 97.408 (1) |
V (Å3) | 1608.19 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.02 |
Crystal size (mm) | 0.20 × 0.17 × 0.15 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.822, 0.862 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14409, 3691, 3064 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.037, 0.113, 1.07 |
No. of reflections | 3691 |
No. of parameters | 289 |
No. of restraints | 25 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.36, −0.45 |
Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998).
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7B···O4i | 0.839 (10) | 1.958 (10) | 2.795 (2) | 175 (3) |
O7—H7A···O2Wii | 0.841 (9) | 1.905 (11) | 2.736 (2) | 170 (3) |
O8—H8A···O3 | 0.827 (9) | 2.294 (19) | 2.904 (2) | 131 (2) |
O8—H8A···O2iii | 0.827 (9) | 2.47 (2) | 3.147 (2) | 140 (2) |
O8—H8B···O2Wiv | 0.829 (10) | 1.962 (11) | 2.788 (2) | 174 (3) |
O9—H9B···O1Wv | 0.833 (10) | 1.946 (14) | 2.743 (2) | 160 (2) |
O9—H9A···N5iii | 0.843 (10) | 2.018 (11) | 2.858 (2) | 174 (3) |
O10—H10A···N5i | 0.842 (10) | 2.058 (11) | 2.895 (2) | 172 (2) |
O10—H10B···O1Wvi | 0.841 (9) | 1.927 (13) | 2.743 (2) | 163 (2) |
O11—H11A···O5vi | 0.835 (10) | 2.079 (19) | 2.828 (2) | 149 (3) |
O11—H11B···O2vii | 0.835 (10) | 1.949 (14) | 2.761 (2) | 164 (3) |
O1W—H1WB···O10i | 0.838 (9) | 2.179 (17) | 2.926 (2) | 148 (3) |
O1W—H1WB···O9i | 0.838 (9) | 2.54 (3) | 3.075 (3) | 123 (3) |
O1W—H1WB···O1i | 0.838 (9) | 2.60 (2) | 3.142 (2) | 124 (2) |
O1W—H1WA···O6viii | 0.837 (10) | 1.916 (12) | 2.736 (2) | 166 (3) |
O2W—H2WA···O6 | 0.844 (10) | 1.892 (10) | 2.734 (2) | 176 (3) |
O2W—H2WB···O7 | 0.849 (10) | 2.053 (13) | 2.859 (2) | 158 (3) |
N3—H3···O4 | 0.851 (10) | 1.947 (11) | 2.790 (2) | 170 (3) |
N4—H4···O3 | 0.853 (10) | 1.979 (11) | 2.829 (2) | 174 (3) |
N6—H6···O1ix | 0.860 (10) | 1.979 (11) | 2.834 (2) | 173 (3) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+3/2; (ii) −x, −y+1, −z+1; (iii) −x+1/2, y−1/2, −z+3/2; (iv) −x, −y, −z+1; (v) x−1, y−1, z; (vi) x−1, y, z; (vii) x−1/2, −y+1/2, z−1/2; (viii) −x+1, −y+1, −z+1; (ix) x+1/2, −y+1/2, z−1/2. |
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Recently we reported a series of one-dimensional helical Ag(I) compounds containing 8-hydroxyquinoline coordinating groups (Cai et al., 2001 and 2003). As a part of the structural studies of the compounds involving the oxygen-nitrogen chelating ligand (Cai et al., 2005), here we report the synthesis and structure of the compound, pentaaqua(1,3,5-triazinanyl-2,4,6-trione)iron(II) 1,3,5-triazinanate-2,4,6-trione dihydrate, namely [Fe(C3H2N3O3)(H2O)5]+(C3H2N3O3)- 2H2O (Scheme 1).
Fig.1 shows that the molecule of [Fe(C3H2N3O3)(H2O)5]+(C3H2N3O3)- 2H2O consists of one cation [Fe(C3H2N3O3)(H2O)5]+, one anion (C3H2N3O3)- and two water molecules. The FeII atom exhibits a FeNO5 octahedral coordination geometry arising from one N-bonded 1,3,5-triazinanyl-2,4,6-trione molecule and five O atoms of water molecules. The uncoordinated 1,3,5-triazinanyl-2,4,6-trione anion and uncoordinated water molecules interact with the cation through O—H···O, O—H···N and N—H···O hydrogen bonds (Table 1), generating a three-dimensional network.