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In the title compound, [Fe(H2O)6](NO3)2·2C6H12N4·4H2O, the ferrous ion is coordinated by six O atoms from six water mol­ecules and is in a slightly distorted octahedral geometry, lying on an inversion center. All the N atoms of the hexa­methyl­enetetr­amine mol­ecules, all the O atoms in the nitrate anions and all the water mol­ecules contribute to the formation of hydrogen bonds. This leads to the formation of a three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680302316X/su6045sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680302316X/su6045Isup2.hkl
Contains datablock I

CCDC reference: 226656

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](O-N) = 0.005 Å
  • R factor = 0.043
  • wR factor = 0.117
  • Data-to-parameter ratio = 9.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.99 PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors .... N1 PLAT731_ALERT_1_B Bond Calc 0.91(7), Rep 0.906(11) ...... 6.36 su-Rat O8 -H10 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.91(7), Rep 0.906(11) ...... 6.36 su-Rat O8 -H10 1.555 1.555
Alert level C REFNR01_ALERT_3_C Ratio of reflections to parameters is < 10 for a centrosymmetric structure sine(theta)/lambda -0.1443 Proportion of unique data used 1.0000 Ratio reflections to parameters 9.1579 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.16 PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 12 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - O1 = 9.53 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - O2 = 7.87 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Fe1 - O3 = 7.76 su PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Fe1 PLAT417_ALERT_2_C Short Inter D-H..H-D H8 .. H10 = 2.14 Ang. PLAT731_ALERT_1_C Bond Calc 0.90(3), Rep 0.904(10) ...... 3.00 su-Rat O1 -H2 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.91(3), Rep 0.905(10) ...... 3.00 su-Rat O2 -H3 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.90(4), Rep 0.903(10) ...... 4.00 su-Rat O2 -H4 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.91(3), Rep 0.911(10) ...... 3.00 su-Rat O3 -H5 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.91(4), Rep 0.907(10) ...... 4.00 su-Rat O7 -H8 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.91(4), Rep 0.912(10) ...... 4.00 su-Rat O8 -H9 1.555 1.555 PLAT732_ALERT_1_C Angle Calc 106(5), Rep 106(2) ...... 2.50 su-Rat H9 -O8 -H10 1.555 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(3), Rep 0.904(10) ...... 3.00 su-Rat O1 -H2 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.91(3), Rep 0.905(10) ...... 3.00 su-Rat O2 -H3 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.90(4), Rep 0.903(10) ...... 4.00 su-Rat O2 -H4 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.91(3), Rep 0.911(10) ...... 3.00 su-Rat O3 -H5 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.91(4), Rep 0.907(10) ...... 4.00 su-Rat O7 -H8 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.91(4), Rep 0.912(10) ...... 4.00 su-Rat O8 -H9 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.91(4), Rep 1.908(13) ...... 3.08 su-Rat H4 -N2 1.555 1.554 PLAT736_ALERT_1_C H...A Calc 1.96(4), Rep 1.965(15) ...... 2.67 su-Rat H5 -O6 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.92(4), Rep 1.917(12) ...... 3.33 su-Rat H8 -O8 1.555 2.666 PLAT736_ALERT_1_C H...A Calc 1.89(4), Rep 1.887(15) ...... 2.67 su-Rat H9 -O5 1.555 1.655 PLAT736_ALERT_1_C H...A Calc 2.03(7), Rep 2.02(2) ...... 3.50 su-Rat H10 -O6 1.555 2.666
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 27 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 21 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Hexaquairon(II) dinitrate bis(dihexamethylenetetramine) tetrahydrate top
Crystal data top
[Fe(H2O)6](NO3)2·2C6H12N4·4H2OZ = 1
Mr = 640.42F(000) = 340
Triclinic, P1Dx = 1.523 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.104 (4) ÅCell parameters from 2715 reflections
b = 9.349 (4) Åθ = 3.0–26.4°
c = 9.700 (4) ŵ = 0.63 mm1
α = 87.743 (5)°T = 298 K
β = 75.674 (4)°Prism, violet
γ = 61.248 (5)°0.33 × 0.25 × 0.18 mm
V = 698.3 (5) Å3
Data collection top
Siemens SMART CCD area-detector
diffractometer
2436 independent reflections
Radiation source: fine-focus sealed tube2261 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.015
φ and ω scansθmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 109
Tmin = 0.820, Tmax = 0.896k = 1011
3689 measured reflectionsl = 1111
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.117All H-atom parameters refined
S = 1.09 w = 1/[σ2(Fo2) + (0.0803P)2 + 0.1663P]
where P = (Fo2 + 2Fc2)/3
2436 reflections(Δ/σ)max = 0.001
266 parametersΔρmax = 0.63 e Å3
15 restraintsΔρmin = 0.46 e Å3
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
Fe10.00000.00000.00000.02441 (18)
N10.0679 (3)0.1779 (4)0.4947 (3)0.0569 (7)
N20.3474 (3)0.1892 (3)0.8379 (3)0.0436 (5)
N30.4508 (3)0.2981 (3)0.6246 (2)0.0448 (5)
N40.5474 (3)0.2929 (3)0.8398 (2)0.0411 (5)
N50.2472 (3)0.4831 (3)0.8372 (2)0.0418 (5)
O10.1077 (2)0.1802 (2)0.1308 (2)0.0432 (4)
O20.2427 (2)0.0491 (2)0.1071 (2)0.0428 (4)
O30.0082 (3)0.1771 (2)0.1272 (2)0.0458 (5)
O40.1005 (5)0.0737 (5)0.5792 (3)0.0997 (10)
O50.0261 (6)0.3204 (4)0.5399 (5)0.1432 (17)
O60.1350 (4)0.1425 (4)0.3645 (3)0.0783 (8)
O70.5191 (3)0.2702 (3)0.3233 (2)0.0647 (6)
O80.8043 (4)0.5914 (4)0.7424 (3)0.0804 (8)
C10.4008 (4)0.1742 (4)0.6798 (3)0.0492 (7)
C20.4944 (4)0.1694 (4)0.8904 (3)0.0454 (6)
C30.2006 (4)0.3560 (4)0.8881 (3)0.0443 (6)
C40.5952 (4)0.2769 (4)0.6819 (3)0.0450 (6)
C50.3028 (4)0.4614 (4)0.6790 (3)0.0464 (6)
C60.3967 (4)0.4562 (3)0.8908 (3)0.0421 (6)
H10.053 (4)0.162 (5)0.2254 (14)0.072 (11)*
H20.2226 (15)0.225 (5)0.123 (3)0.078 (12)*
H30.309 (5)0.122 (4)0.185 (3)0.089 (13)*
H40.265 (5)0.035 (3)0.119 (4)0.097 (15)*
H50.024 (5)0.157 (4)0.211 (2)0.066 (10)*
H60.073 (4)0.2884 (14)0.131 (3)0.072 (11)*
H70.503 (4)0.273 (5)0.4195 (12)0.071 (11)*
H80.413 (3)0.322 (5)0.306 (4)0.087 (14)*
H90.857 (7)0.497 (4)0.684 (5)0.117 (19)*
H100.831 (11)0.662 (6)0.690 (6)0.23 (4)*
H110.309 (4)0.178 (4)0.638 (3)0.050 (8)*
H120.498 (5)0.061 (5)0.638 (4)0.057 (9)*
H130.454 (4)0.188 (4)1.008 (3)0.051 (8)*
H140.601 (5)0.046 (5)0.850 (4)0.061 (9)*
H150.167 (4)0.366 (4)0.999 (4)0.049 (8)*
H160.097 (4)0.374 (3)0.851 (3)0.039 (7)*
H170.697 (4)0.167 (4)0.651 (3)0.049 (8)*
H180.620 (4)0.373 (4)0.650 (3)0.048 (8)*
H190.205 (5)0.479 (5)0.635 (4)0.065 (10)*
H200.328 (4)0.551 (4)0.644 (3)0.052 (8)*
H210.356 (4)0.463 (3)1.002 (3)0.041 (7)*
H220.425 (4)0.540 (4)0.861 (3)0.048 (8)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0236 (3)0.0241 (3)0.0244 (3)0.01027 (19)0.00718 (17)0.00218 (17)
N10.0503 (15)0.0641 (18)0.0500 (15)0.0221 (13)0.0139 (12)0.0010 (13)
N20.0418 (12)0.0410 (12)0.0501 (13)0.0227 (10)0.0098 (10)0.0016 (10)
N30.0449 (13)0.0502 (14)0.0376 (12)0.0216 (11)0.0102 (10)0.0012 (10)
N40.0379 (11)0.0438 (12)0.0450 (12)0.0203 (10)0.0160 (9)0.0071 (10)
N50.0401 (12)0.0377 (12)0.0429 (12)0.0141 (10)0.0129 (9)0.0009 (9)
O10.0395 (10)0.0471 (11)0.0424 (10)0.0190 (9)0.0157 (8)0.0123 (8)
O20.0369 (10)0.0419 (11)0.0454 (11)0.0197 (8)0.0019 (8)0.0020 (8)
O30.0535 (12)0.0360 (10)0.0465 (11)0.0161 (9)0.0222 (9)0.0007 (8)
O40.117 (3)0.106 (2)0.0615 (17)0.043 (2)0.0243 (17)0.0243 (17)
O50.150 (4)0.069 (2)0.128 (3)0.009 (2)0.010 (3)0.023 (2)
O60.0853 (18)0.095 (2)0.0471 (13)0.0388 (16)0.0160 (12)0.0033 (13)
O70.0604 (15)0.0710 (16)0.0436 (12)0.0231 (12)0.0002 (10)0.0054 (11)
O80.0822 (19)0.082 (2)0.0692 (17)0.0351 (17)0.0173 (14)0.0053 (15)
C10.0513 (17)0.0489 (17)0.0498 (16)0.0270 (14)0.0096 (13)0.0082 (13)
C20.0439 (15)0.0406 (15)0.0511 (16)0.0189 (12)0.0164 (12)0.0109 (12)
C30.0352 (14)0.0470 (16)0.0488 (16)0.0196 (12)0.0080 (12)0.0011 (12)
C40.0377 (15)0.0507 (17)0.0451 (15)0.0218 (13)0.0074 (12)0.0034 (12)
C50.0466 (16)0.0480 (16)0.0440 (15)0.0195 (13)0.0191 (12)0.0092 (12)
C60.0466 (15)0.0410 (15)0.0444 (15)0.0232 (12)0.0167 (12)0.0022 (11)
Geometric parameters (Å, º) top
Fe1—O2i2.0242 (19)O1—H20.904 (10)
Fe1—O22.0242 (19)O2—H30.905 (10)
Fe1—O32.0658 (19)O2—H40.903 (10)
Fe1—O3i2.0658 (19)O3—H50.911 (10)
Fe1—O1i2.0660 (18)O3—H60.913 (10)
Fe1—O12.0660 (18)O7—H70.906 (10)
N1—O51.209 (4)O7—H80.907 (10)
N1—O41.220 (4)O8—H90.912 (10)
N1—O61.238 (4)O8—H100.906 (11)
N2—C21.474 (4)C1—H111.00 (3)
N2—C31.479 (4)C1—H121.01 (4)
N2—C11.480 (4)C2—H131.10 (3)
N3—C51.469 (4)C2—H141.09 (4)
N3—C11.474 (4)C3—H151.04 (3)
N3—C41.476 (4)C3—H161.03 (3)
N4—C61.472 (4)C4—H170.98 (3)
N4—C21.477 (4)C4—H181.05 (3)
N4—C41.478 (4)C5—H191.02 (4)
N5—C31.473 (4)C5—H201.00 (4)
N5—C51.481 (4)C6—H211.04 (3)
N5—C61.482 (3)C6—H220.95 (3)
O1—H10.907 (10)
O2i—Fe1—O2180.00 (10)H7—O7—H8107 (2)
O2i—Fe1—O392.38 (8)H9—O8—H10106 (2)
O2—Fe1—O387.62 (8)N3—C1—N2112.0 (2)
O2i—Fe1—O3i87.62 (8)N3—C1—H11111.2 (19)
O2—Fe1—O3i92.38 (8)N2—C1—H11111.4 (18)
O3—Fe1—O3i180.00 (11)N3—C1—H12110 (2)
O2i—Fe1—O1i88.59 (8)N2—C1—H12112.7 (19)
O2—Fe1—O1i91.41 (8)H11—C1—H1299 (3)
O3—Fe1—O1i87.60 (8)N2—C2—N4111.7 (2)
O3i—Fe1—O1i92.40 (8)N2—C2—H13109.1 (16)
O2i—Fe1—O191.41 (8)N4—C2—H13106.5 (17)
O2—Fe1—O188.59 (8)N2—C2—H14106.4 (18)
O3—Fe1—O192.40 (8)N4—C2—H14110.4 (19)
O3i—Fe1—O187.60 (8)H13—C2—H14113 (2)
O1i—Fe1—O1180.0N5—C3—N2111.7 (2)
O5—N1—O4119.0 (4)N5—C3—H15109.4 (18)
O5—N1—O6119.1 (4)N2—C3—H15107.5 (18)
O4—N1—O6121.8 (3)N5—C3—H16107.7 (16)
C2—N2—C3108.3 (2)N2—C3—H16110.0 (16)
C2—N2—C1108.0 (2)H15—C3—H16111 (2)
C3—N2—C1108.4 (2)N3—C4—N4111.9 (2)
C5—N3—C1108.5 (2)N3—C4—H17111.1 (19)
C5—N3—C4108.0 (2)N4—C4—H17106.7 (18)
C1—N3—C4108.2 (2)N3—C4—H18106.6 (17)
C6—N4—C2107.9 (2)N4—C4—H18106.7 (17)
C6—N4—C4108.4 (2)H17—C4—H18114 (3)
C2—N4—C4108.5 (2)N3—C5—N5112.1 (2)
C3—N5—C5108.4 (2)N3—C5—H19108 (2)
C3—N5—C6107.7 (2)N5—C5—H19112 (2)
C5—N5—C6108.4 (2)N3—C5—H20112.3 (19)
Fe1—O1—H1118 (2)N5—C5—H20108.6 (18)
Fe1—O1—H2118 (2)H19—C5—H20103 (3)
H1—O1—H2107 (2)N4—C6—N5111.8 (2)
Fe1—O2—H3125 (3)N4—C6—H21108.1 (16)
Fe1—O2—H4118 (3)N5—C6—H21106.3 (16)
H3—O2—H4107 (2)N4—C6—H22111.2 (19)
Fe1—O3—H5123 (2)N5—C6—H22108.2 (19)
Fe1—O3—H6129 (2)H21—C6—H22111 (2)
H5—O3—H6105 (2)
C5—N3—C1—N258.2 (3)C5—N3—C4—N459.0 (3)
C4—N3—C1—N258.8 (3)C1—N3—C4—N458.2 (3)
C2—N2—C1—N359.1 (3)C6—N4—C4—N358.8 (3)
C3—N2—C1—N358.1 (3)C2—N4—C4—N358.1 (3)
C3—N2—C2—N458.6 (3)C1—N3—C5—N558.3 (3)
C1—N2—C2—N458.7 (3)C4—N3—C5—N558.8 (3)
C6—N4—C2—N258.9 (3)C3—N5—C5—N358.5 (3)
C4—N4—C2—N258.4 (3)C6—N5—C5—N358.2 (3)
C5—N5—C3—N258.3 (3)C2—N4—C6—N559.4 (3)
C6—N5—C3—N258.9 (3)C4—N4—C6—N558.0 (3)
C2—N2—C3—N558.8 (3)C3—N5—C6—N459.5 (3)
C1—N2—C3—N558.2 (3)C5—N5—C6—N457.7 (3)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O4ii0.91 (1)1.98 (1)2.874 (4)167 (3)
O1—H2···N4iii0.90 (1)2.00 (2)2.879 (3)165 (3)
O2—H3···O7iv0.91 (1)1.79 (2)2.674 (3)167 (4)
O2—H4···N2v0.90 (1)1.91 (1)2.803 (3)171 (4)
O3—H5···O60.91 (1)1.97 (2)2.850 (3)163 (3)
O3—H6···N5vi0.91 (1)1.93 (1)2.830 (3)168 (4)
O7—H7···N30.91 (1)1.92 (1)2.828 (3)175 (3)
O7—H8···O8vii0.91 (1)1.92 (1)2.819 (4)174 (4)
O8—H9···O5viii0.91 (1)1.89 (2)2.791 (5)171 (5)
O8—H10···O6vii0.91 (1)2.02 (2)2.899 (5)162 (6)
Symmetry codes: (ii) x, y, z+1; (iii) x+1, y, z+1; (iv) x+1, y, z; (v) x, y, z1; (vi) x, y+1, z+1; (vii) x+1, y+1, z+1; (viii) x+1, y, z.
 

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