Hex­aqua­iron(II) dinitrate bis­(dihexa­methyl­enetetr­amine) tetrahydrate

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.

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

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Computing details

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

Crystal data

[Fe(H2O)6](NO3)2·2C6H12N4·4H2O	Z = 1
Mr = 640.42	F(000) = 340
Triclinic, P1	Dx = 1.523 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.104 (4) Å	Cell parameters from 2715 reflections
b = 9.349 (4) Å	θ = 3.0–26.4°
c = 9.700 (4) Å	µ = 0.63 mm^−1
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) Å^3

Data collection

Siemens SMART CCD area-detector diffractometer	2436 independent reflections
Radiation source: fine-focus sealed tube	2261 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.015
φ and ω scans	θmax = 25.0°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→9
Tmin = 0.820, Tmax = 0.896	k = −10→11
3689 measured reflections	l = −11→11

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.043	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.117	All H-atom parameters refined
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0803P)^2 + 0.1663P] where P = (Fo^2 + 2Fc^2)/3
2436 reflections	(Δ/σ)max = 0.001
266 parameters	Δρmax = 0.63 e Å^−3
15 restraints	Δρmin = −0.46 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.0000	0.0000	0.0000	0.02441 (18)
N1	0.0679 (3)	0.1779 (4)	0.4947 (3)	0.0569 (7)
N2	0.3474 (3)	0.1892 (3)	0.8379 (3)	0.0436 (5)
N3	0.4508 (3)	0.2981 (3)	0.6246 (2)	0.0448 (5)
N4	0.5474 (3)	0.2929 (3)	0.8398 (2)	0.0411 (5)
N5	0.2472 (3)	0.4831 (3)	0.8372 (2)	0.0418 (5)
O1	0.1077 (2)	−0.1802 (2)	0.1308 (2)	0.0432 (4)
O2	0.2427 (2)	−0.0491 (2)	−0.1071 (2)	0.0428 (4)
O3	−0.0082 (3)	0.1771 (2)	0.1272 (2)	0.0458 (5)
O4	0.1005 (5)	0.0737 (5)	0.5792 (3)	0.0997 (10)
O5	−0.0261 (6)	0.3204 (4)	0.5399 (5)	0.1432 (17)
O6	0.1350 (4)	0.1425 (4)	0.3645 (3)	0.0783 (8)
O7	0.5191 (3)	0.2702 (3)	0.3233 (2)	0.0647 (6)
O8	0.8043 (4)	0.5914 (4)	0.7424 (3)	0.0804 (8)
C1	0.4008 (4)	0.1742 (4)	0.6798 (3)	0.0492 (7)
C2	0.4944 (4)	0.1694 (4)	0.8904 (3)	0.0454 (6)
C3	0.2006 (4)	0.3560 (4)	0.8881 (3)	0.0443 (6)
C4	0.5952 (4)	0.2769 (4)	0.6819 (3)	0.0450 (6)
C5	0.3028 (4)	0.4614 (4)	0.6790 (3)	0.0464 (6)
C6	0.3967 (4)	0.4562 (3)	0.8908 (3)	0.0421 (6)
H1	0.053 (4)	−0.162 (5)	0.2254 (14)	0.072 (11)*
H2	0.2226 (15)	−0.225 (5)	0.123 (3)	0.078 (12)*
H3	0.309 (5)	−0.122 (4)	−0.185 (3)	0.089 (13)*
H4	0.265 (5)	0.035 (3)	−0.119 (4)	0.097 (15)*
H5	0.024 (5)	0.157 (4)	0.211 (2)	0.066 (10)*
H6	−0.073 (4)	0.2884 (14)	0.131 (3)	0.072 (11)*
H7	0.503 (4)	0.273 (5)	0.4195 (12)	0.071 (11)*
H8	0.413 (3)	0.322 (5)	0.306 (4)	0.087 (14)*
H9	0.857 (7)	0.497 (4)	0.684 (5)	0.117 (19)*
H10	0.831 (11)	0.662 (6)	0.690 (6)	0.23 (4)*
H11	0.309 (4)	0.178 (4)	0.638 (3)	0.050 (8)*
H12	0.498 (5)	0.061 (5)	0.638 (4)	0.057 (9)*
H13	0.454 (4)	0.188 (4)	1.008 (3)	0.051 (8)*
H14	0.601 (5)	0.046 (5)	0.850 (4)	0.061 (9)*
H15	0.167 (4)	0.366 (4)	0.999 (4)	0.049 (8)*
H16	0.097 (4)	0.374 (3)	0.851 (3)	0.039 (7)*
H17	0.697 (4)	0.167 (4)	0.651 (3)	0.049 (8)*
H18	0.620 (4)	0.373 (4)	0.650 (3)	0.048 (8)*
H19	0.205 (5)	0.479 (5)	0.635 (4)	0.065 (10)*
H20	0.328 (4)	0.551 (4)	0.644 (3)	0.052 (8)*
H21	0.356 (4)	0.463 (3)	1.002 (3)	0.041 (7)*
H22	0.425 (4)	0.540 (4)	0.861 (3)	0.048 (8)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0236 (3)	0.0241 (3)	0.0244 (3)	−0.01027 (19)	−0.00718 (17)	0.00218 (17)
N1	0.0503 (15)	0.0641 (18)	0.0500 (15)	−0.0221 (13)	−0.0139 (12)	−0.0010 (13)
N2	0.0418 (12)	0.0410 (12)	0.0501 (13)	−0.0227 (10)	−0.0098 (10)	0.0016 (10)
N3	0.0449 (13)	0.0502 (14)	0.0376 (12)	−0.0216 (11)	−0.0102 (10)	−0.0012 (10)
N4	0.0379 (11)	0.0438 (12)	0.0450 (12)	−0.0203 (10)	−0.0160 (9)	0.0071 (10)
N5	0.0401 (12)	0.0377 (12)	0.0429 (12)	−0.0141 (10)	−0.0129 (9)	0.0009 (9)
O1	0.0395 (10)	0.0471 (11)	0.0424 (10)	−0.0190 (9)	−0.0157 (8)	0.0123 (8)
O2	0.0369 (10)	0.0419 (11)	0.0454 (11)	−0.0197 (8)	−0.0019 (8)	−0.0020 (8)
O3	0.0535 (12)	0.0360 (10)	0.0465 (11)	−0.0161 (9)	−0.0222 (9)	−0.0007 (8)
O4	0.117 (3)	0.106 (2)	0.0615 (17)	−0.043 (2)	−0.0243 (17)	0.0243 (17)
O5	0.150 (4)	0.069 (2)	0.128 (3)	−0.009 (2)	0.010 (3)	−0.023 (2)
O6	0.0853 (18)	0.095 (2)	0.0471 (13)	−0.0388 (16)	−0.0160 (12)	0.0033 (13)
O7	0.0604 (15)	0.0710 (16)	0.0436 (12)	−0.0231 (12)	0.0002 (10)	−0.0054 (11)
O8	0.0822 (19)	0.082 (2)	0.0692 (17)	−0.0351 (17)	−0.0173 (14)	0.0053 (15)
C1	0.0513 (17)	0.0489 (17)	0.0498 (16)	−0.0270 (14)	−0.0096 (13)	−0.0082 (13)
C2	0.0439 (15)	0.0406 (15)	0.0511 (16)	−0.0189 (12)	−0.0164 (12)	0.0109 (12)
C3	0.0352 (14)	0.0470 (16)	0.0488 (16)	−0.0196 (12)	−0.0080 (12)	−0.0011 (12)
C4	0.0377 (15)	0.0507 (17)	0.0451 (15)	−0.0218 (13)	−0.0074 (12)	0.0034 (12)
C5	0.0466 (16)	0.0480 (16)	0.0440 (15)	−0.0195 (13)	−0.0191 (12)	0.0092 (12)
C6	0.0466 (15)	0.0410 (15)	0.0444 (15)	−0.0232 (12)	−0.0167 (12)	0.0022 (11)

Geometric parameters (Å, º)

Fe1—O2^i	2.0242 (19)	O1—H2	0.904 (10)
Fe1—O2	2.0242 (19)	O2—H3	0.905 (10)
Fe1—O3	2.0658 (19)	O2—H4	0.903 (10)
Fe1—O3^i	2.0658 (19)	O3—H5	0.911 (10)
Fe1—O1^i	2.0660 (18)	O3—H6	0.913 (10)
Fe1—O1	2.0660 (18)	O7—H7	0.906 (10)
N1—O5	1.209 (4)	O7—H8	0.907 (10)
N1—O4	1.220 (4)	O8—H9	0.912 (10)
N1—O6	1.238 (4)	O8—H10	0.906 (11)
N2—C2	1.474 (4)	C1—H11	1.00 (3)
N2—C3	1.479 (4)	C1—H12	1.01 (4)
N2—C1	1.480 (4)	C2—H13	1.10 (3)
N3—C5	1.469 (4)	C2—H14	1.09 (4)
N3—C1	1.474 (4)	C3—H15	1.04 (3)
N3—C4	1.476 (4)	C3—H16	1.03 (3)
N4—C6	1.472 (4)	C4—H17	0.98 (3)
N4—C2	1.477 (4)	C4—H18	1.05 (3)
N4—C4	1.478 (4)	C5—H19	1.02 (4)
N5—C3	1.473 (4)	C5—H20	1.00 (4)
N5—C5	1.481 (4)	C6—H21	1.04 (3)
N5—C6	1.482 (3)	C6—H22	0.95 (3)
O1—H1	0.907 (10)
O2^i—Fe1—O2	180.00 (10)	H7—O7—H8	107 (2)
O2^i—Fe1—O3	92.38 (8)	H9—O8—H10	106 (2)
O2—Fe1—O3	87.62 (8)	N3—C1—N2	112.0 (2)
O2^i—Fe1—O3^i	87.62 (8)	N3—C1—H11	111.2 (19)
O2—Fe1—O3^i	92.38 (8)	N2—C1—H11	111.4 (18)
O3—Fe1—O3^i	180.00 (11)	N3—C1—H12	110 (2)
O2^i—Fe1—O1^i	88.59 (8)	N2—C1—H12	112.7 (19)
O2—Fe1—O1^i	91.41 (8)	H11—C1—H12	99 (3)
O3—Fe1—O1^i	87.60 (8)	N2—C2—N4	111.7 (2)
O3^i—Fe1—O1^i	92.40 (8)	N2—C2—H13	109.1 (16)
O2^i—Fe1—O1	91.41 (8)	N4—C2—H13	106.5 (17)
O2—Fe1—O1	88.59 (8)	N2—C2—H14	106.4 (18)
O3—Fe1—O1	92.40 (8)	N4—C2—H14	110.4 (19)
O3^i—Fe1—O1	87.60 (8)	H13—C2—H14	113 (2)
O1^i—Fe1—O1	180.0	N5—C3—N2	111.7 (2)
O5—N1—O4	119.0 (4)	N5—C3—H15	109.4 (18)
O5—N1—O6	119.1 (4)	N2—C3—H15	107.5 (18)
O4—N1—O6	121.8 (3)	N5—C3—H16	107.7 (16)
C2—N2—C3	108.3 (2)	N2—C3—H16	110.0 (16)
C2—N2—C1	108.0 (2)	H15—C3—H16	111 (2)
C3—N2—C1	108.4 (2)	N3—C4—N4	111.9 (2)
C5—N3—C1	108.5 (2)	N3—C4—H17	111.1 (19)
C5—N3—C4	108.0 (2)	N4—C4—H17	106.7 (18)
C1—N3—C4	108.2 (2)	N3—C4—H18	106.6 (17)
C6—N4—C2	107.9 (2)	N4—C4—H18	106.7 (17)
C6—N4—C4	108.4 (2)	H17—C4—H18	114 (3)
C2—N4—C4	108.5 (2)	N3—C5—N5	112.1 (2)
C3—N5—C5	108.4 (2)	N3—C5—H19	108 (2)
C3—N5—C6	107.7 (2)	N5—C5—H19	112 (2)
C5—N5—C6	108.4 (2)	N3—C5—H20	112.3 (19)
Fe1—O1—H1	118 (2)	N5—C5—H20	108.6 (18)
Fe1—O1—H2	118 (2)	H19—C5—H20	103 (3)
H1—O1—H2	107 (2)	N4—C6—N5	111.8 (2)
Fe1—O2—H3	125 (3)	N4—C6—H21	108.1 (16)
Fe1—O2—H4	118 (3)	N5—C6—H21	106.3 (16)
H3—O2—H4	107 (2)	N4—C6—H22	111.2 (19)
Fe1—O3—H5	123 (2)	N5—C6—H22	108.2 (19)
Fe1—O3—H6	129 (2)	H21—C6—H22	111 (2)
H5—O3—H6	105 (2)
C5—N3—C1—N2	−58.2 (3)	C5—N3—C4—N4	59.0 (3)
C4—N3—C1—N2	58.8 (3)	C1—N3—C4—N4	−58.2 (3)
C2—N2—C1—N3	−59.1 (3)	C6—N4—C4—N3	−58.8 (3)
C3—N2—C1—N3	58.1 (3)	C2—N4—C4—N3	58.1 (3)
C3—N2—C2—N4	−58.6 (3)	C1—N3—C5—N5	58.3 (3)
C1—N2—C2—N4	58.7 (3)	C4—N3—C5—N5	−58.8 (3)
C6—N4—C2—N2	58.9 (3)	C3—N5—C5—N3	−58.5 (3)
C4—N4—C2—N2	−58.4 (3)	C6—N5—C5—N3	58.2 (3)
C5—N5—C3—N2	58.3 (3)	C2—N4—C6—N5	−59.4 (3)
C6—N5—C3—N2	−58.9 (3)	C4—N4—C6—N5	58.0 (3)
C2—N2—C3—N5	58.8 (3)	C3—N5—C6—N4	59.5 (3)
C1—N2—C3—N5	−58.2 (3)	C5—N5—C6—N4	−57.7 (3)

Symmetry code: (i) −x, −y, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O4^ii	0.91 (1)	1.98 (1)	2.874 (4)	167 (3)
O1—H2···N4^iii	0.90 (1)	2.00 (2)	2.879 (3)	165 (3)
O2—H3···O7^iv	0.91 (1)	1.79 (2)	2.674 (3)	167 (4)
O2—H4···N2^v	0.90 (1)	1.91 (1)	2.803 (3)	171 (4)
O3—H5···O6	0.91 (1)	1.97 (2)	2.850 (3)	163 (3)
O3—H6···N5^vi	0.91 (1)	1.93 (1)	2.830 (3)	168 (4)
O7—H7···N3	0.91 (1)	1.92 (1)	2.828 (3)	175 (3)
O7—H8···O8^vii	0.91 (1)	1.92 (1)	2.819 (4)	174 (4)
O8—H9···O5^viii	0.91 (1)	1.89 (2)	2.791 (5)	171 (5)
O8—H10···O6^vii	0.91 (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, z−1; (vi) −x, −y+1, −z+1; (vii) −x+1, −y+1, −z+1; (viii) x+1, y, z.