Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
In the title compound, [Fe(C3H2N3O3)(H2O)5](C3H2N3O3)·2H2O, the FeII atom exhibits an 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, generating a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807045060/ww2093sup1.cif
Contains datablocks I, Iyp10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807045060/ww2093Isup2.hkl
Contains datablock I

CCDC reference: 663632

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](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

Comment top

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.

Related literature top

For general background, see: Cai et al. (2001). For related structures, see: Cai et al. (2003). For related literature, see: Cai, et al. (2005).

Experimental top

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%.

Refinement top

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.

Structure description top

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).

Computing details top

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).

Figures top
[Figure 1] Fig. 1. The structure of title molecule, with its atom-numbering scheme, is shown at the 50% probability level.
Pentaaqua(isocyanurato)iron(II) isocyanurate dihydrate top
Crystal data top
[Fe(C3H2N3O3)(H2O)5](C3H2N3O3)·2H2OF(000) = 904
Mr = 438.11Dx = 1.809 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 4778 reflections
a = 14.0563 (2) Åθ = 2.4–27.4°
b = 6.6947 (1) ŵ = 1.02 mm1
c = 17.2336 (3) ÅT = 298 K
β = 97.408 (1)°Block, green
V = 1608.19 (4) Å30.20 × 0.17 × 0.15 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
3691 independent reflections
Radiation source: fine-focus sealed tube3064 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
φ and ω scansθmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1817
Tmin = 0.822, Tmax = 0.862k = 86
14409 measured reflectionsl = 2222
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.113H 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 parametersΔρmax = 0.36 e Å3
25 restraintsΔρmin = 0.45 e Å3
Crystal data top
[Fe(C3H2N3O3)(H2O)5](C3H2N3O3)·2H2OV = 1608.19 (4) Å3
Mr = 438.11Z = 4
Monoclinic, P21/nMo Kα radiation
a = 14.0563 (2) ŵ = 1.02 mm1
b = 6.6947 (1) ÅT = 298 K
c = 17.2336 (3) Å0.20 × 0.17 × 0.15 mm
β = 97.408 (1)°
Data collection top
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 = 0.862Rint = 0.028
14409 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03725 restraints
wR(F2) = 0.113H atoms treated by a mixture of independent and constrained refinement
S = 1.07Δρmax = 0.36 e Å3
3691 reflectionsΔρmin = 0.45 e Å3
289 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
Fe10.05822 (2)0.17964 (5)0.678490 (17)0.02687 (13)
O10.01859 (11)0.1853 (3)0.87539 (9)0.0296 (4)
O20.30290 (12)0.2819 (3)0.93035 (10)0.0421 (5)
O30.17061 (11)0.1783 (3)0.68074 (9)0.0327 (4)
O40.41363 (11)0.1655 (3)0.75242 (8)0.0289 (4)
O50.60977 (11)0.2088 (3)0.56299 (10)0.0377 (4)
O60.28965 (12)0.2944 (3)0.50276 (10)0.0433 (5)
O70.00205 (11)0.4449 (3)0.62062 (9)0.0302 (4)
H7B0.0276 (17)0.510 (3)0.6578 (11)0.045*
H7A0.0367 (17)0.512 (3)0.5867 (11)0.045*
O80.00260 (12)0.0127 (3)0.59652 (10)0.0372 (4)
H8A0.0619 (7)0.014 (4)0.6028 (18)0.056*
H8B0.0266 (16)0.107 (3)0.5730 (18)0.056*
O90.13082 (12)0.0603 (3)0.72935 (10)0.0329 (4)
H9B0.1713 (16)0.122 (4)0.6988 (13)0.049*
H9A0.0971 (17)0.129 (3)0.7635 (13)0.049*
O100.13586 (11)0.3992 (3)0.74129 (9)0.0284 (3)
H10A0.0988 (15)0.472 (3)0.7713 (13)0.043*
H10B0.1783 (14)0.459 (3)0.7112 (13)0.043*
O110.18778 (12)0.1871 (3)0.59092 (10)0.0404 (5)
H11A0.2439 (11)0.197 (5)0.6014 (16)0.061*
H11B0.179 (2)0.201 (5)0.5442 (8)0.061*
O1W0.74356 (12)0.6644 (3)0.65640 (9)0.0329 (4)
H1WB0.6986 (14)0.692 (5)0.6821 (12)0.049*
H1WA0.7299 (18)0.657 (5)0.6077 (6)0.049*
O2W0.09420 (12)0.3139 (3)0.49336 (10)0.0339 (4)
H2WA0.1543 (8)0.301 (5)0.4958 (15)0.051*
H2WB0.0736 (17)0.326 (5)0.5373 (10)0.051*
N10.06881 (12)0.1824 (3)0.77285 (10)0.0205 (4)
N20.14088 (12)0.2369 (3)0.90343 (10)0.0247 (4)
H20.1357 (19)0.244 (4)0.9520 (7)0.030*
N30.23620 (13)0.2187 (3)0.80582 (11)0.0286 (4)
H30.2910 (11)0.217 (4)0.7898 (16)0.034*
N40.35144 (13)0.2299 (3)0.62800 (10)0.0246 (4)
H40.2955 (10)0.223 (4)0.6421 (15)0.029*
N50.51845 (12)0.1830 (3)0.66238 (10)0.0232 (4)
N60.45021 (13)0.2501 (3)0.53267 (10)0.0274 (4)
H60.4638 (19)0.262 (4)0.4856 (8)0.033*
C10.05928 (15)0.2003 (3)0.85001 (12)0.0207 (4)
C20.23144 (15)0.2485 (4)0.88340 (12)0.0264 (5)
C30.15702 (15)0.1924 (3)0.75000 (12)0.0220 (4)
C40.42988 (14)0.1913 (3)0.68387 (12)0.0213 (4)
C50.53042 (15)0.2133 (3)0.58650 (12)0.0242 (4)
C60.35972 (15)0.2595 (4)0.55118 (12)0.0256 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.02585 (19)0.0331 (2)0.02092 (18)0.00181 (13)0.00026 (12)0.00010 (12)
O10.0202 (7)0.0491 (10)0.0200 (7)0.0022 (7)0.0045 (6)0.0003 (7)
O20.0236 (8)0.0810 (14)0.0206 (8)0.0096 (9)0.0013 (6)0.0031 (8)
O30.0228 (8)0.0586 (12)0.0171 (7)0.0006 (7)0.0034 (6)0.0039 (7)
O40.0259 (8)0.0444 (10)0.0171 (7)0.0045 (7)0.0052 (6)0.0065 (6)
O50.0188 (8)0.0717 (13)0.0231 (8)0.0025 (8)0.0048 (6)0.0027 (8)
O60.0200 (8)0.0872 (16)0.0216 (8)0.0053 (8)0.0016 (6)0.0065 (9)
O70.0311 (8)0.0352 (9)0.0231 (8)0.0038 (7)0.0002 (6)0.0045 (7)
O80.0258 (8)0.0480 (11)0.0378 (9)0.0018 (8)0.0038 (7)0.0163 (8)
O90.0293 (8)0.0351 (9)0.0322 (9)0.0057 (7)0.0047 (7)0.0081 (7)
O100.0248 (8)0.0321 (9)0.0267 (8)0.0017 (7)0.0021 (6)0.0028 (7)
O110.0227 (8)0.0769 (14)0.0206 (8)0.0017 (9)0.0007 (6)0.0016 (8)
O1W0.0266 (8)0.0496 (11)0.0224 (8)0.0031 (7)0.0031 (6)0.0009 (7)
O2W0.0244 (8)0.0484 (11)0.0289 (8)0.0003 (8)0.0034 (6)0.0008 (7)
N10.0170 (8)0.0287 (9)0.0156 (8)0.0003 (7)0.0019 (6)0.0002 (7)
N20.0206 (9)0.0389 (11)0.0146 (8)0.0012 (8)0.0026 (7)0.0025 (8)
N30.0160 (8)0.0514 (13)0.0187 (9)0.0008 (8)0.0031 (7)0.0031 (8)
N40.0160 (8)0.0397 (11)0.0186 (8)0.0010 (8)0.0042 (7)0.0019 (8)
N50.0192 (8)0.0322 (10)0.0180 (8)0.0016 (7)0.0018 (6)0.0010 (7)
N60.0204 (9)0.0475 (12)0.0146 (8)0.0008 (8)0.0029 (7)0.0006 (8)
C10.0199 (9)0.0238 (11)0.0182 (9)0.0004 (8)0.0015 (7)0.0007 (8)
C20.0236 (10)0.0370 (12)0.0183 (10)0.0012 (9)0.0012 (8)0.0009 (9)
C30.0207 (10)0.0275 (11)0.0175 (9)0.0004 (8)0.0010 (7)0.0008 (8)
C40.0198 (10)0.0242 (11)0.0199 (10)0.0007 (8)0.0021 (8)0.0005 (8)
C50.0187 (9)0.0338 (12)0.0198 (10)0.0002 (8)0.0022 (8)0.0001 (8)
C60.0191 (9)0.0386 (12)0.0189 (10)0.0008 (9)0.0015 (8)0.0010 (9)
Geometric parameters (Å, º) top
Fe1—O92.1495 (17)O1W—H1WA0.837 (10)
Fe1—O82.1671 (17)O2W—H2WA0.844 (10)
Fe1—O102.1973 (16)O2W—H2WB0.849 (10)
Fe1—O112.2109 (16)N1—C31.350 (3)
Fe1—O72.2303 (17)N1—C11.359 (3)
Fe1—N12.2549 (16)N2—C21.363 (3)
O1—C11.234 (3)N2—C11.397 (3)
O2—C21.226 (3)N2—H20.851 (10)
O3—C31.237 (3)N3—C21.362 (3)
O4—C41.244 (2)N3—C31.385 (3)
O5—C51.235 (3)N3—H30.851 (10)
O6—C61.228 (3)N4—C61.358 (3)
O7—H7B0.839 (10)N4—C41.391 (3)
O7—H7A0.841 (9)N4—H40.853 (10)
O8—H8A0.827 (9)N5—C41.345 (3)
O8—H8B0.829 (10)N5—C51.355 (3)
O9—H9B0.833 (10)N6—C61.352 (3)
O9—H9A0.843 (10)N6—C51.387 (3)
O10—H10A0.842 (10)N6—H60.860 (10)
O10—H10B0.841 (9)C3—O31.237 (3)
O11—H11A0.835 (10)C4—O41.244 (2)
O11—H11B0.835 (10)C6—O61.228 (3)
O1W—H1WB0.838 (9)
O9—Fe1—O893.99 (8)C1—N1—Fe1122.52 (14)
O9—Fe1—O1090.40 (7)C2—N2—C1123.87 (18)
O8—Fe1—O10168.93 (6)C2—N2—H2116.6 (18)
O9—Fe1—O1184.41 (7)C1—N2—H2119.4 (18)
O8—Fe1—O1185.87 (7)C2—N3—C3124.30 (19)
O10—Fe1—O1184.46 (7)C2—N3—H3118.8 (19)
O9—Fe1—O7172.46 (6)C3—N3—H3116.9 (19)
O8—Fe1—O789.41 (7)C6—N4—C4122.80 (19)
O10—Fe1—O785.09 (7)C6—N4—H4118.9 (18)
O11—Fe1—O789.12 (7)C4—N4—H4118.0 (18)
O9—Fe1—O7172.46 (6)C4—N5—C5119.60 (18)
O8—Fe1—O789.41 (7)C6—N6—C5123.98 (18)
O10—Fe1—O785.09 (7)C6—N6—H6123.2 (19)
O11—Fe1—O789.12 (7)C5—N6—H6112.8 (19)
O9—Fe1—N194.91 (6)O1—C1—N1122.93 (19)
O8—Fe1—N197.63 (6)O1—C1—N2118.11 (19)
O10—Fe1—N192.10 (6)N1—C1—N2118.96 (18)
O11—Fe1—N1176.48 (7)O2—C2—N3122.3 (2)
O7—Fe1—N191.31 (6)O2—C2—N2123.7 (2)
O7—Fe1—N191.31 (6)N3—C2—N2113.95 (18)
Fe1—O7—H7B103.8 (18)O3—C3—N1122.67 (18)
Fe1—O7—H7A122.0 (19)O3—C3—N1122.67 (18)
H7B—O7—H7A116.2 (14)O3—C3—N3118.01 (19)
Fe1—O8—H8A113.3 (19)O3—C3—N3118.01 (19)
Fe1—O8—H8B124 (2)N1—C3—N3119.32 (18)
H8A—O8—H8B119.0 (15)O4—C4—N5123.06 (18)
Fe1—O9—H9B115.7 (19)O4—C4—N5123.06 (18)
Fe1—O9—H9A116.1 (19)O4—C4—N4117.18 (19)
H9B—O9—H9A116.6 (14)O4—C4—N4117.18 (19)
Fe1—O10—H10A112.6 (18)N5—C4—N4119.76 (18)
Fe1—O10—H10B112.0 (18)O5—C5—N5122.86 (19)
H10A—O10—H10B115.8 (14)O5—C5—N6118.40 (19)
Fe1—O11—H11A125 (2)N5—C5—N6118.74 (19)
Fe1—O11—H11B117 (2)O6—C6—N6123.0 (2)
H11A—O11—H11B117.4 (15)O6—C6—N6123.0 (2)
H1WB—O1W—H1WA116.8 (14)O6—C6—N4121.9 (2)
H2WA—O2W—H2WB114.9 (14)O6—C6—N4121.9 (2)
C3—N1—C1119.42 (17)N6—C6—N4115.12 (19)
C3—N1—Fe1117.50 (13)
O9—Fe1—N1—C3134.41 (15)C1—N1—C3—O3179.6 (2)
O8—Fe1—N1—C339.71 (16)Fe1—N1—C3—O38.0 (3)
O10—Fe1—N1—C3135.00 (15)C1—N1—C3—N30.6 (3)
O11—Fe1—N1—C3146.9 (11)Fe1—N1—C3—N3172.28 (16)
O7—Fe1—N1—C349.86 (15)C2—N3—C3—O3175.8 (2)
O7—Fe1—N1—C349.86 (15)C2—N3—C3—O3175.8 (2)
O9—Fe1—N1—C154.23 (17)C2—N3—C3—N14.4 (3)
O8—Fe1—N1—C1148.93 (16)C5—N5—C4—O4179.8 (2)
O10—Fe1—N1—C136.36 (16)C5—N5—C4—O4179.8 (2)
O11—Fe1—N1—C124.5 (13)C5—N5—C4—N40.3 (3)
O7—Fe1—N1—C1121.50 (16)C6—N4—C4—O4179.6 (2)
O7—Fe1—N1—C1121.50 (16)C6—N4—C4—O4179.6 (2)
C3—N1—C1—O1177.2 (2)C6—N4—C4—N50.3 (3)
Fe1—N1—C1—O111.6 (3)C4—N5—C5—O5179.6 (2)
C3—N1—C1—N22.6 (3)C4—N5—C5—N60.8 (3)
Fe1—N1—C1—N2168.57 (15)C6—N6—C5—O5179.7 (2)
C2—N2—C1—O1177.2 (2)C6—N6—C5—N50.6 (4)
C2—N2—C1—N12.7 (3)C5—N6—C6—O6179.2 (2)
C3—N3—C2—O2176.0 (2)C5—N6—C6—O6179.2 (2)
C3—N3—C2—N24.3 (4)C5—N6—C6—N40.1 (4)
C1—N2—C2—O2179.5 (2)C4—N4—C6—O6179.7 (2)
C1—N2—C2—N30.7 (3)C4—N4—C6—O6179.7 (2)
C1—N1—C3—O3179.6 (2)C4—N4—C6—N60.4 (3)
Fe1—N1—C3—O38.0 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7B···O4i0.84 (1)1.96 (1)2.795 (2)175 (3)
O7—H7A···O2Wii0.84 (1)1.91 (1)2.736 (2)170 (3)
O8—H8A···O30.83 (1)2.29 (2)2.904 (2)131 (2)
O8—H8A···O2iii0.83 (1)2.47 (2)3.147 (2)140 (2)
O8—H8B···O2Wiv0.83 (1)1.96 (1)2.788 (2)174 (3)
O9—H9B···O1Wv0.83 (1)1.95 (1)2.743 (2)160 (2)
O9—H9A···N5iii0.84 (1)2.02 (1)2.858 (2)174 (3)
O10—H10A···N5i0.84 (1)2.06 (1)2.895 (2)172 (2)
O10—H10B···O1Wvi0.84 (1)1.93 (1)2.743 (2)163 (2)
O11—H11A···O5vi0.84 (1)2.08 (2)2.828 (2)149 (3)
O11—H11B···O2vii0.84 (1)1.95 (1)2.761 (2)164 (3)
O1W—H1WB···O10i0.84 (1)2.18 (2)2.926 (2)148 (3)
O1W—H1WB···O9i0.84 (1)2.54 (3)3.075 (3)123 (3)
O1W—H1WB···O1i0.84 (1)2.60 (2)3.142 (2)124 (2)
O1W—H1WA···O6viii0.84 (1)1.92 (1)2.736 (2)166 (3)
O2W—H2WA···O60.84 (1)1.89 (1)2.734 (2)176 (3)
O2W—H2WB···O70.85 (1)2.05 (1)2.859 (2)158 (3)
N3—H3···O40.85 (1)1.95 (1)2.790 (2)170 (3)
N4—H4···O30.85 (1)1.98 (1)2.829 (2)174 (3)
N6—H6···O1ix0.86 (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, y1/2, z+3/2; (iv) x, y, z+1; (v) x1, y1, z; (vi) x1, y, z; (vii) x1/2, y+1/2, z1/2; (viii) x+1, y+1, z+1; (ix) x+1/2, y+1/2, z1/2.

Experimental details

Crystal data
Chemical formula[Fe(C3H2N3O3)(H2O)5](C3H2N3O3)·2H2O
Mr438.11
Crystal system, space groupMonoclinic, P21/n
Temperature (K)298
a, b, c (Å)14.0563 (2), 6.6947 (1), 17.2336 (3)
β (°) 97.408 (1)
V3)1608.19 (4)
Z4
Radiation typeMo Kα
µ (mm1)1.02
Crystal size (mm)0.20 × 0.17 × 0.15
Data collection
DiffractometerBruker SMART CCD area-detector
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.822, 0.862
No. of measured, independent and
observed [I > 2σ(I)] reflections
14409, 3691, 3064
Rint0.028
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.113, 1.07
No. of reflections3691
No. of parameters289
No. of restraints25
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.36, 0.45

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1998).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7B···O4i0.839 (10)1.958 (10)2.795 (2)175 (3)
O7—H7A···O2Wii0.841 (9)1.905 (11)2.736 (2)170 (3)
O8—H8A···O30.827 (9)2.294 (19)2.904 (2)131 (2)
O8—H8A···O2iii0.827 (9)2.47 (2)3.147 (2)140 (2)
O8—H8B···O2Wiv0.829 (10)1.962 (11)2.788 (2)174 (3)
O9—H9B···O1Wv0.833 (10)1.946 (14)2.743 (2)160 (2)
O9—H9A···N5iii0.843 (10)2.018 (11)2.858 (2)174 (3)
O10—H10A···N5i0.842 (10)2.058 (11)2.895 (2)172 (2)
O10—H10B···O1Wvi0.841 (9)1.927 (13)2.743 (2)163 (2)
O11—H11A···O5vi0.835 (10)2.079 (19)2.828 (2)149 (3)
O11—H11B···O2vii0.835 (10)1.949 (14)2.761 (2)164 (3)
O1W—H1WB···O10i0.838 (9)2.179 (17)2.926 (2)148 (3)
O1W—H1WB···O9i0.838 (9)2.54 (3)3.075 (3)123 (3)
O1W—H1WB···O1i0.838 (9)2.60 (2)3.142 (2)124 (2)
O1W—H1WA···O6viii0.837 (10)1.916 (12)2.736 (2)166 (3)
O2W—H2WA···O60.844 (10)1.892 (10)2.734 (2)176 (3)
O2W—H2WB···O70.849 (10)2.053 (13)2.859 (2)158 (3)
N3—H3···O40.851 (10)1.947 (11)2.790 (2)170 (3)
N4—H4···O30.853 (10)1.979 (11)2.829 (2)174 (3)
N6—H6···O1ix0.860 (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, y1/2, z+3/2; (iv) x, y, z+1; (v) x1, y1, z; (vi) x1, y, z; (vii) x1/2, y+1/2, z1/2; (viii) x+1, y+1, z+1; (ix) x+1/2, y+1/2, z1/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

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