Crystal structure of the co-crystal fac-tri­aqua­tris(thio­cyanato-κN)iron(III)–2,3-di­methyl­pyrazine (1/3)

The Fe^III complex located on a threefold rotation axis links with di­methyl­perazine mol­ecules via O—H...N hydrogen bonds,forming a three-dimensional supra­molecular framework.

Key indicators

• Single-crystal X-ray study
• T = 133 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.038
• wR factor = 0.070
• Data-to-parameter ratio = 15.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT090_ALERT_3_C Poor Data / Parameter Ratio (Zmax > 18) ........       8.70 Note
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............     0.0077 Ang.
PLAT735_ALERT_1_C D-H     Calc     0.80(7), Rep     0.80(3) ......          2 su-Rat
              O1   -H1A     1.555   1.555                #         26
PLAT736_ALERT_1_C H...A   Calc     1.95(7), Rep     1.95(3) ......        2.3 su-Rat
              H1A  -N2      1.555   1.555                #         26

Alert level G
PLAT005_ALERT_5_G No _iucr_refine_instructions_details  in the CIF     Please Do !
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          3 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   4 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   2 ALERT level G = General information/check it is not something unexpected

   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
   3 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA (Stoe & Cie, 2002); data reduction: X-RED (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: publCIF (Westrip, 2010).

fac-Triaquatris(thiocyanato-κN)iron(III)–2,3-dimethylpyrazine (1/3)

Crystal data

[Fe(NCS)3(H2O)3]·3C6H8N2	F(000) = 1902
Mr = 608.57	Dx = 1.384 Mg m^−3
Trigonal, R3c	Mo Kα radiation, λ = 0.71073 Å
a = 16.9383 (12) Å	µ = 0.77 mm^−1
c = 17.6259 (13) Å	T = 133 K
V = 4379.5 (7) Å^3	Block, red
Z = 6	0.16 × 0.12 × 0.1 mm

Data collection

Stoe IPDS II diffractometer	1716 reflections with I > 2σ(I)
φ scans and ω scans with κ offset	Rint = 0.058
Absorption correction: numerical (X-RED; Stoe & Cie, 2002)	θmax = 26.8°, θmin = 2.4°
Tmin = 0.908, Tmax = 0.939	h = −18→21
5784 measured reflections	k = −21→15
1903 independent reflections	l = −18→22

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.038	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.070	w = 1/[σ^2(Fo^2) + (0.0297P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max < 0.001
1903 reflections	Δρmax = 0.27 e Å^−3
120 parameters	Δρmin = −0.28 e Å^−3
3 restraints	Absolute structure: Flack x determined using 685 quotients [(I^+)-(I^-)]/[(I^+)+(I^-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: −0.03 (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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe1	0.3333	0.6667	0.99891 (7)	0.0201 (2)
S1	0.29300 (8)	0.86373 (8)	1.16318 (7)	0.0300 (3)
N1	0.2860 (3)	0.7347 (3)	1.0611 (2)	0.0297 (9)
O1	0.2256 (2)	0.62277 (19)	0.92686 (19)	0.0221 (6)
C1	0.2893 (3)	0.7891 (3)	1.1041 (3)	0.0238 (9)
N2	0.0562 (2)	0.5854 (2)	0.9750 (2)	0.0250 (8)
N3	−0.1220 (2)	0.5016 (2)	1.0276 (2)	0.0254 (8)
C2	0.0336 (3)	0.5471 (3)	1.0439 (3)	0.0299 (10)
H2	0.0796	0.5481	1.0753	0.036*
C3	−0.0543 (3)	0.5064 (3)	1.0704 (3)	0.0288 (10)
H3	−0.0674	0.4812	1.1201	0.035*
C4	−0.1008 (3)	0.5385 (3)	0.9586 (2)	0.0235 (9)
C5	−0.0099 (3)	0.5815 (3)	0.9318 (3)	0.0229 (9)
C6	−0.1766 (3)	0.5322 (3)	0.9107 (3)	0.0322 (10)
H6A	−0.2345	0.4977	0.9379	0.048*
H6B	−0.1795	0.5010	0.8630	0.048*
H6C	−0.1655	0.5936	0.8996	0.048*
C7	0.0144 (3)	0.6246 (3)	0.8553 (3)	0.0304 (10)
H7A	0.0795	0.6484	0.8459	0.046*
H7B	0.0012	0.6747	0.8531	0.046*
H7C	−0.0214	0.5791	0.8166	0.046*
H1A	0.179 (3)	0.617 (5)	0.943 (4)	0.080*
H1B	0.206 (5)	0.572 (3)	0.912 (4)	0.080*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.0197 (3)	0.0197 (3)	0.0209 (5)	0.00986 (13)	0.000	0.000
S1	0.0320 (6)	0.0293 (5)	0.0316 (6)	0.0175 (5)	0.0009 (5)	−0.0061 (5)
N1	0.030 (2)	0.031 (2)	0.029 (2)	0.0157 (18)	0.0031 (17)	−0.0024 (18)
O1	0.0180 (14)	0.0201 (14)	0.0283 (17)	0.0096 (13)	−0.0011 (13)	−0.0021 (13)
C1	0.022 (2)	0.030 (2)	0.022 (2)	0.0141 (18)	0.0019 (17)	0.0053 (18)
N2	0.0234 (18)	0.0234 (17)	0.028 (2)	0.0119 (15)	−0.0004 (16)	−0.0026 (15)
N3	0.0236 (17)	0.0233 (17)	0.029 (2)	0.0113 (15)	0.0027 (15)	0.0001 (15)
C2	0.027 (2)	0.037 (2)	0.030 (3)	0.019 (2)	−0.0040 (19)	−0.001 (2)
C3	0.032 (2)	0.029 (2)	0.028 (3)	0.018 (2)	0.0022 (19)	0.0030 (19)
C4	0.021 (2)	0.023 (2)	0.027 (2)	0.0113 (16)	0.0008 (18)	−0.0022 (18)
C5	0.023 (2)	0.0203 (19)	0.027 (2)	0.0121 (17)	0.0023 (17)	−0.0028 (17)
C6	0.027 (2)	0.036 (3)	0.035 (3)	0.017 (2)	−0.002 (2)	−0.002 (2)
C7	0.026 (2)	0.037 (2)	0.028 (3)	0.016 (2)	0.0020 (19)	0.0020 (19)

Geometric parameters (Å, º)

Fe1—N1	2.025 (4)	N3—C4	1.333 (6)
Fe1—N1^i	2.025 (4)	C2—H2	0.9500
Fe1—N1^ii	2.025 (4)	C2—C3	1.372 (6)
Fe1—O1	2.034 (3)	C3—H3	0.9500
Fe1—O1^i	2.034 (3)	C4—C5	1.415 (6)
Fe1—O1^ii	2.034 (3)	C4—C6	1.495 (6)
S1—C1	1.615 (5)	C5—C7	1.491 (6)
N1—C1	1.172 (6)	C6—H6A	0.9800
O1—H1A	0.80 (3)	C6—H6B	0.9800
O1—H1B	0.80 (3)	C6—H6C	0.9800
N2—C2	1.339 (6)	C7—H7A	0.9800
N2—C5	1.329 (5)	C7—H7B	0.9800
N3—C3	1.340 (6)	C7—H7C	0.9800
N1—Fe1—N1^i	93.42 (17)	N2—C2—C3	121.9 (4)
N1—Fe1—N1^ii	93.42 (17)	C3—C2—H2	119.0
N1^i—Fe1—N1^ii	93.42 (16)	N3—C3—C2	121.2 (5)
N1—Fe1—O1^ii	90.67 (14)	N3—C3—H3	119.4
N1^ii—Fe1—O1^ii	90.47 (14)	C2—C3—H3	119.4
N1^ii—Fe1—O1^i	90.67 (14)	N3—C4—C5	120.9 (4)
N1^i—Fe1—O1^ii	174.17 (17)	N3—C4—C6	117.6 (4)
N1—Fe1—O1	90.47 (14)	C5—C4—C6	121.5 (4)
N1^i—Fe1—O1^i	90.47 (14)	N2—C5—C4	120.5 (4)
N1^ii—Fe1—O1	174.17 (17)	N2—C5—C7	118.3 (4)
N1^i—Fe1—O1	90.67 (14)	C4—C5—C7	121.2 (4)
N1—Fe1—O1^i	174.17 (17)	C4—C6—H6A	109.5
O1—Fe1—O1^ii	85.15 (14)	C4—C6—H6B	109.5
O1^ii—Fe1—O1^i	85.15 (14)	C4—C6—H6C	109.5
O1—Fe1—O1^i	85.15 (14)	H6A—C6—H6B	109.5
C1—N1—Fe1	157.0 (4)	H6A—C6—H6C	109.5
Fe1—O1—H1A	118 (6)	H6B—C6—H6C	109.5
Fe1—O1—H1B	115 (6)	C5—C7—H7A	109.5
H1A—O1—H1B	98 (7)	C5—C7—H7B	109.5
N1—C1—S1	179.5 (4)	C5—C7—H7C	109.5
C5—N2—C2	117.7 (4)	H7A—C7—H7B	109.5
C4—N3—C3	117.7 (4)	H7A—C7—H7C	109.5
N2—C2—H2	119.0	H7B—C7—H7C	109.5
N2—C2—C3—N3	1.5 (7)	C3—N3—C4—C6	179.4 (4)
N3—C4—C5—N2	0.4 (6)	C4—N3—C3—C2	−0.7 (7)
N3—C4—C5—C7	−178.7 (4)	C5—N2—C2—C3	−1.2 (6)
C2—N2—C5—C4	0.3 (6)	C6—C4—C5—N2	−179.2 (4)
C2—N2—C5—C7	179.5 (4)	C6—C4—C5—C7	1.7 (6)
C3—N3—C4—C5	−0.2 (6)

Symmetry codes: (i) −y+1, x−y+1, z; (ii) −x+y, −x+1, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···N2	0.80 (3)	1.95 (3)	2.745 (4)	172 (8)