Crystal structure, synthesis and thermal properties of bis­(4-benzoyl­pyridine-κN)bis­(iso­thio­cyanato-κN)bis­(methanol-κN)iron(II)

Wellm, C.; Näther, C.

doi:10.1107/S2056989020001152

Crystal structure, synthesis and thermal properties of bis(4-benzoylpyridine-κN)bis(isothiocyanato-κN)bis(methanol-κN)iron(II)

In the crystal structure of the title compound, the Fe^II cations are octahedrally coordinated into discrete complexes that are linked into layers via intermolecular O—H

O hydrogen bonding.

Keywords: crystal structure; iron(II) thiocyanate; solvate; discrete complex; hydrogen bonding.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989020001152/lh5944sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989020001152/lh5944Isup2.hkl Contains datablock I
	Tagged Image Format File (TIF) image https://doi.org/10.1107/S2056989020001152/lh5944sup3.tif FigureS1. Experimental powder patterns of the title compound (A), of the title compound kept at room temperature for two months (B), of the residue obtained after the first mass loss in a TG measurements of the aforementioned aged sample (C), of the residue obtained after the first mass loss in a TG measurements of the title compound (D), of the residue obtained after the first mass loss in a TG measurement of \[Fe(NCS)2(4-benzoylpyridine)4\] (E),of the residue obtained after the first mass loss in a TG measurement of \[Mn(NCS)2(4-benzoylpyridine)4\] (F) and the calculated patterns of \[Co(NCS)2(4-benzoylpyridine)2\] (G) and \[Cd(NCS)2(4-benzoylpyridine)2\] (H).
	Tagged Image Format File (TIF) image https://doi.org/10.1107/S2056989020001152/lh5944sup4.tif FigureS2. IR spectra of the of the title compound (A), of the title compound kept at room temperature for two months (B), of the residue obtained after the first mass loss in a TG measurements of the aforementioned aged sample (C), of the residue obtained after the first mass loss in a TG measurements of the title compound (D), of the residue obtained after the first mass loss in a TG measurement of \[Fe(NCS)2(4-benzoylpyridine)4\] (E), of the residue obtained after the first mass loss in a TG measurement of \[Mn(NCS)2(4-benzoylpyridine)4\] (F), of \[Co(NCS)2(4-benzoylpyridine)2\] (G) and of \[Cd(NCS)2(4-benzoylpyridine)2\] (H).
	Tagged Image Format File (TIF) image https://doi.org/10.1107/S2056989020001152/lh5944sup5.tif FigureS3. DTG, TG and DTA curves of the title compound at a heating rate of 1 C/min with the experimental mass loss in % and peak temperatures in C.

CCDC reference: 1980369

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Key indicators

Single-crystal X-ray study
T = 200 K
Mean (C-C) = 0.002 Å
R factor = 0.037
wR factor = 0.104
Data-to-parameter ratio = 19.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT048_ALERT_1_C MoietyFormula Not Given (or Incomplete) ........     Please Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          5 Report
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          4 Note

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          1 Report
PLAT230_ALERT_2_G Hirshfeld Test Diff for    S1       --C1       .        8.9 s.u.
PLAT794_ALERT_5_G Tentative Bond Valency for Fe1       (II)      .       2.04 Info
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          2 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         23 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          7 Info

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

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   2 ALERT type 5 Informative message, check

Computing details top

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis(4-benzoylpyridine-κN)bis(isothiocyanato-κN)bis(methanol-κN)iron(II) top

Crystal data top

[Fe(NCS)₂(C₁₂H₉NO)₂(CH₄O)₂]	F(000) = 624
M_r = 602.50	D_x = 1.416 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 12.1111 (8) Å	Cell parameters from 19758 reflections
b = 7.2385 (3) Å	θ = 2.5–28.1°
c = 16.1716 (12) Å	µ = 0.72 mm⁻¹
β = 94.730 (8)°	T = 200 K
V = 1412.87 (15) Å³	Block, light yellow
Z = 2	0.12 × 0.08 × 0.06 mm

Data collection top

STOE IPDS-1 diffractometer	3012 reflections with I > 2σ(I)
Phi scans	R_int = 0.038
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 2008)	θ_max = 28.1°, θ_min = 2.5°
T_min = 0.834, T_max = 0.973	h = −16→16
19758 measured reflections	k = −9→9
3422 independent reflections	l = −21→21

Refinement top

Refinement on F²	Hydrogen site location: mixed
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.037	w = 1/[σ²(F_o²) + (0.0694P)² + 0.430P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.104	(Δ/σ)_max < 0.001
S = 1.03	Δρ_max = 0.36 e Å⁻³
3422 reflections	Δρ_min = −0.51 e Å⁻³
179 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.033 (3)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Fe1	0.0000	0.0000	0.5000	0.02289 (12)
N1	−0.11410 (12)	0.1948 (2)	0.45147 (10)	0.0371 (3)
C1	−0.19503 (13)	0.2661 (2)	0.42451 (10)	0.0281 (3)
S1	−0.30854 (4)	0.36594 (7)	0.38796 (3)	0.04332 (15)
N11	0.13430 (11)	0.14836 (18)	0.44116 (8)	0.0258 (3)
C11	0.21746 (13)	0.0529 (2)	0.41200 (10)	0.0277 (3)
H11	0.2228	−0.0756	0.4236	0.033*
C12	0.29604 (13)	0.1328 (2)	0.36572 (9)	0.0270 (3)
H12	0.3521	0.0594	0.3442	0.032*
C13	0.29163 (12)	0.3217 (2)	0.35128 (9)	0.0248 (3)
C14	0.20752 (13)	0.4230 (2)	0.38307 (10)	0.0298 (3)
H14	0.2031	0.5529	0.3752	0.036*
C15	0.13013 (13)	0.3312 (2)	0.42649 (10)	0.0301 (3)
H15	0.0715	0.4006	0.4468	0.036*
C16	0.37576 (13)	0.4045 (2)	0.29890 (9)	0.0270 (3)
C17	0.43593 (12)	0.5737 (2)	0.32626 (10)	0.0264 (3)
C18	0.49691 (14)	0.6691 (2)	0.27018 (11)	0.0346 (4)
H18	0.4953	0.6297	0.2141	0.042*
C19	0.55965 (16)	0.8209 (3)	0.29656 (14)	0.0433 (4)
H19	0.6001	0.8871	0.2583	0.052*
C20	0.56366 (16)	0.8766 (3)	0.37870 (15)	0.0450 (5)
H20	0.6074	0.9802	0.3967	0.054*
C21	0.50409 (16)	0.7819 (3)	0.43474 (13)	0.0399 (4)
H21	0.5075	0.8202	0.4911	0.048*
C22	0.43953 (13)	0.6315 (2)	0.40878 (10)	0.0310 (3)
H22	0.3978	0.5679	0.4471	0.037*
O11	0.39260 (11)	0.32281 (19)	0.23480 (7)	0.0377 (3)
C23	0.1420 (2)	0.2043 (4)	0.64942 (14)	0.0593 (6)
H23A	0.1367	0.2868	0.6970	0.089*
H23B	0.1741	0.0861	0.6686	0.089*
H23C	0.1892	0.2611	0.6101	0.089*
O1	0.03337 (11)	0.1736 (2)	0.60921 (7)	0.0384 (3)
H1	−0.0132	0.1745	0.6449	0.058*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.01880 (17)	0.02661 (18)	0.02419 (17)	0.00042 (10)	0.00730 (11)	0.00354 (10)
N1	0.0278 (7)	0.0385 (8)	0.0454 (8)	0.0046 (6)	0.0063 (6)	0.0136 (6)
C1	0.0294 (7)	0.0260 (7)	0.0300 (7)	−0.0012 (6)	0.0080 (6)	0.0049 (6)
S1	0.0333 (2)	0.0431 (3)	0.0525 (3)	0.00961 (18)	−0.00278 (19)	0.0089 (2)
N11	0.0226 (6)	0.0289 (6)	0.0271 (6)	−0.0030 (5)	0.0089 (5)	0.0019 (5)
C11	0.0258 (7)	0.0269 (7)	0.0316 (7)	−0.0003 (6)	0.0096 (6)	0.0031 (6)
C12	0.0232 (7)	0.0290 (7)	0.0301 (7)	0.0008 (6)	0.0104 (6)	0.0018 (6)
C13	0.0222 (7)	0.0290 (7)	0.0238 (6)	−0.0045 (6)	0.0054 (5)	0.0017 (5)
C14	0.0286 (8)	0.0247 (7)	0.0375 (8)	−0.0009 (6)	0.0104 (6)	0.0014 (6)
C15	0.0259 (7)	0.0277 (7)	0.0382 (8)	−0.0002 (6)	0.0129 (6)	−0.0008 (6)
C16	0.0239 (7)	0.0313 (7)	0.0264 (7)	−0.0013 (6)	0.0063 (5)	0.0059 (6)
C17	0.0199 (6)	0.0281 (7)	0.0313 (7)	0.0001 (6)	0.0034 (5)	0.0058 (6)
C18	0.0310 (8)	0.0350 (8)	0.0388 (8)	−0.0036 (7)	0.0082 (7)	0.0086 (7)
C19	0.0333 (9)	0.0351 (9)	0.0625 (12)	−0.0087 (7)	0.0109 (8)	0.0111 (8)
C20	0.0318 (9)	0.0300 (8)	0.0730 (14)	−0.0049 (7)	0.0034 (9)	−0.0040 (8)
C21	0.0357 (9)	0.0342 (9)	0.0494 (10)	0.0004 (7)	0.0008 (8)	−0.0081 (8)
C22	0.0274 (7)	0.0316 (8)	0.0341 (8)	−0.0002 (6)	0.0035 (6)	0.0004 (6)
O11	0.0429 (7)	0.0434 (7)	0.0288 (6)	−0.0114 (6)	0.0157 (5)	−0.0027 (5)
C23	0.0489 (12)	0.0856 (17)	0.0439 (11)	−0.0272 (12)	0.0077 (9)	−0.0189 (11)
O1	0.0357 (6)	0.0517 (8)	0.0293 (6)	−0.0068 (6)	0.0123 (5)	−0.0080 (5)

Geometric parameters (Å, º) top

Fe1—N1ⁱ	2.0823 (15)	C16—O11	1.225 (2)
Fe1—N1	2.0823 (15)	C16—C17	1.474 (2)
Fe1—O1ⁱ	2.1780 (12)	C17—C22	1.396 (2)
Fe1—O1	2.1780 (12)	C17—C18	1.398 (2)
Fe1—N11ⁱ	2.2270 (12)	C18—C19	1.383 (3)
Fe1—N11	2.2270 (12)	C18—H18	0.9500
N1—C1	1.160 (2)	C19—C20	1.385 (3)
C1—S1	1.6209 (17)	C19—H19	0.9500
N11—C11	1.339 (2)	C20—C21	1.386 (3)
N11—C15	1.345 (2)	C20—H20	0.9500
C11—C12	1.385 (2)	C21—C22	1.385 (2)
C11—H11	0.9500	C21—H21	0.9500
C12—C13	1.388 (2)	C22—H22	0.9500
C12—H12	0.9500	C23—O1	1.436 (3)
C13—C14	1.388 (2)	C23—H23A	0.9800
C13—C16	1.502 (2)	C23—H23B	0.9800
C14—C15	1.386 (2)	C23—H23C	0.9800
C14—H14	0.9500	O1—H1	0.8401
C15—H15	0.9500

N1ⁱ—Fe1—N1	180.00 (8)	N11—C15—H15	118.5
N1ⁱ—Fe1—O1ⁱ	89.31 (6)	C14—C15—H15	118.5
N1—Fe1—O1ⁱ	90.69 (6)	O11—C16—C17	122.83 (14)
N1ⁱ—Fe1—O1	90.69 (6)	O11—C16—C13	116.92 (14)
N1—Fe1—O1	89.31 (6)	C17—C16—C13	120.23 (13)
O1ⁱ—Fe1—O1	180.00 (4)	C22—C17—C18	119.69 (15)
N1ⁱ—Fe1—N11ⁱ	89.87 (5)	C22—C17—C16	120.78 (14)
N1—Fe1—N11ⁱ	90.13 (5)	C18—C17—C16	119.34 (15)
O1ⁱ—Fe1—N11ⁱ	88.57 (5)	C19—C18—C17	119.90 (17)
O1—Fe1—N11ⁱ	91.43 (5)	C19—C18—H18	120.1
N1ⁱ—Fe1—N11	90.13 (5)	C17—C18—H18	120.1
N1—Fe1—N11	89.87 (5)	C18—C19—C20	120.13 (17)
O1ⁱ—Fe1—N11	91.43 (5)	C18—C19—H19	119.9
O1—Fe1—N11	88.57 (5)	C20—C19—H19	119.9
N11ⁱ—Fe1—N11	180.0	C19—C20—C21	120.28 (17)
C1—N1—Fe1	163.04 (14)	C19—C20—H20	119.9
N1—C1—S1	179.32 (16)	C21—C20—H20	119.9
C11—N11—C15	117.66 (13)	C22—C21—C20	120.13 (18)
C11—N11—Fe1	119.92 (10)	C22—C21—H21	119.9
C15—N11—Fe1	122.13 (10)	C20—C21—H21	119.9
N11—C11—C12	123.04 (15)	C21—C22—C17	119.86 (16)
N11—C11—H11	118.5	C21—C22—H22	120.1
C12—C11—H11	118.5	C17—C22—H22	120.1
C11—C12—C13	118.94 (14)	O1—C23—H23A	109.5
C11—C12—H12	120.5	O1—C23—H23B	109.5
C13—C12—H12	120.5	H23A—C23—H23B	109.5
C12—C13—C14	118.52 (13)	O1—C23—H23C	109.5
C12—C13—C16	117.99 (14)	H23A—C23—H23C	109.5
C14—C13—C16	123.44 (14)	H23B—C23—H23C	109.5
C15—C14—C13	118.83 (15)	C23—O1—Fe1	123.95 (12)
C15—C14—H14	120.6	C23—O1—H1	109.2
C13—C14—H14	120.6	Fe1—O1—H1	118.2
N11—C15—C14	122.95 (14)

Symmetry code: (i) −x, −y, −z+1.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O11ⁱⁱ	0.84	1.92	2.7574 (16)	174

Symmetry code: (ii) x−1/2, −y+1/2, z+1/2.

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Crystal structure, synthesis and thermal properties of bis­(4-benzoyl­pyridine-κN)bis­(iso­thio­cyanato-κN)bis­(methanol-κN)iron(II)

Supporting information

Key indicators

checkCIF/PLATON results

Crystal structure, synthesis and thermal properties of bis(4-benzoylpyridine-κN)bis(isothiocyanato-κN)bis(methanol-κN)iron(II)