Literature DB >> 21582078

catena-Poly[bis-[cis-dipyrimidine-trans-dithio-cyanato-iron(II)]-di-μ-pyrimidine-[trans-dithio-cyanato-iron(II)]-di-μ-pyrimidine].

Mario Wriedt¹, Sina Sellmer, Inke Jess, Christian Näther.

Abstract

In the crystal structure of the title compound, [Fe(3)(NCS)(6)(C(4)H(4)N(2))(8)](n), each iron(II) cation is coordinated by four N-bonded pyrimidine ligands and two N-bonded thio-cyanate anions in a distorted octa-hedral environment. The asymmetric unit consists of one iron cation located on a crystallographic center of inversion, as well as one iron cation, three thio-cyanate anions and four pyrimidine ligands occupying general positions. The structure consists of square secondary building units (SBUs) with an Fe atom at each corner, which are μ-N(1):N(3)-bridged by the pyrimidine ligands. The SBUs are linked into infinite chains running in the c-axis direction via common opposite corners.

Entities: Chemical Disease Species

Year: 2009 PMID： 21582078 PMCID： PMC2968508 DOI： 10.1107/S1600536809005509

Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN： 1600-5368

Related literature

For related pyrimidine structures, see: Lloret et al. (1998 ▶); Näther et al. (2007 ▶); Näther & Jess (2004 ▶). For general background, see: Näther & Greve (2003 ▶); Näther, Wriedt & Jess (2003 ▶); Wriedt et al. (2008 ▶, 2009 ▶).

Experimental

Crystal data

[Fe3(NCS)6(C4H4N2)8] M = 1156.77 Monoclinic, a = 18.256 (1) Å b = 16.2855 (9) Å c = 8.2765 (4) Å β = 100.042 (7)° V = 2423.0 (2) Å3 Z = 2 Mo Kα radiation μ = 1.20 mm−1 T = 170 K 0.12 × 0.10 × 0.07 mm

Data collection

Stoe IPDS-1 diffractometer Absorption correction: numerical (X-SHAPE and X-RED32; Stoe, 2008 ▶) T min = 0.859, T max = 0.912 20463 measured reflections 4615 independent reflections 3795 reflections with I > 2σ(I) R int = 0.064

Refinement

R[F 2 > 2σ(F 2)] = 0.051 wR(F 2) = 0.124 S = 1.13 4615 reflections 314 parameters H-atom parameters constrained Δρmax = 0.95 e Å−3 Δρmin = −0.41 e Å−3 Data collection: X-AREA (Stoe, 2008 ▶); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: XP in SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: XCIF in SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809005509/im2102sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809005509/im2102Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Fe₃(NCS)₆(C₄H₄N₂)₈]	F(000) = 1176
M_r = 1156.77	D_x = 1.586 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 8000 reflections
a = 18.256 (1) Å	θ = 8.3–27.2°
b = 16.2855 (9) Å	µ = 1.20 mm⁻¹
c = 8.2765 (4) Å	T = 170 K
β = 100.042 (7)°	Block, red
V = 2423.0 (2) Å³	0.12 × 0.10 × 0.07 mm
Z = 2

Stoe IPDS-1 diffractometer	4615 independent reflections
Radiation source: fine-focus sealed tube	3795 reflections with I > 2σ(I)
graphite	R_int = 0.064
φ scans	θ_max = 26.0°, θ_min = 2.6°
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe, 2008)	h = −22→22
T_min = 0.859, T_max = 0.912	k = −20→20
20463 measured reflections	l = −10→10

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.051	H-atom parameters constrained
wR(F²) = 0.124	w = 1/[σ²(F_o²) + (0.0419P)² + 8.0294P] where P = (F_o² + 2F_c²)/3
S = 1.13	(Δ/σ)_max < 0.001
4615 reflections	Δρ_max = 0.95 e Å⁻³
314 parameters	Δρ_min = −0.41 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0024 (5)

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.

	x	y	z	U_iso*/U_eq
Fe1	0.26416 (3)	0.48712 (3)	0.61108 (6)	0.01115 (16)
Fe2	0.0000	0.5000	1.0000	0.01002 (18)
N41	0.26059 (19)	0.5829 (2)	0.7749 (4)	0.0202 (7)
C41	0.2859 (2)	0.6276 (2)	0.8790 (5)	0.0182 (8)
S41	0.32547 (8)	0.68848 (8)	1.02316 (17)	0.0418 (4)
N51	0.26521 (18)	0.3912 (2)	0.4439 (4)	0.0184 (7)
C51	0.26229 (19)	0.3726 (2)	0.3063 (5)	0.0127 (7)
S51	0.25824 (6)	0.35068 (7)	0.11413 (12)	0.0241 (3)
N61	0.00127 (18)	0.5933 (2)	0.8299 (4)	0.0167 (7)
C61	0.0140 (2)	0.6208 (2)	0.7072 (5)	0.0146 (8)
S61	0.03129 (7)	0.65765 (7)	0.53635 (14)	0.0292 (3)
N1	0.17147 (16)	0.42202 (19)	0.7062 (4)	0.0131 (6)
N2	0.07898 (17)	0.42630 (19)	0.8767 (4)	0.0131 (6)
C1	0.12769 (19)	0.4614 (2)	0.7952 (4)	0.0130 (7)
H1	0.1317	0.5195	0.8008	0.016*
C2	0.0754 (2)	0.3440 (2)	0.8720 (5)	0.0165 (8)
H2	0.0432	0.3166	0.9330	0.020*
C3	0.1170 (2)	0.2978 (2)	0.7813 (5)	0.0179 (8)
H3	0.1133	0.2397	0.7768	0.021*
C4	0.1643 (2)	0.3399 (2)	0.6977 (5)	0.0164 (8)
H4	0.1927	0.3099	0.6320	0.020*
N11	0.36347 (17)	0.5483 (2)	0.5208 (4)	0.0157 (7)
N12	0.4695 (2)	0.6360 (2)	0.5800 (5)	0.0264 (8)
C11	0.4082 (2)	0.6011 (3)	0.6157 (5)	0.0212 (9)
H11	0.3949	0.6149	0.7183	0.025*
C12	0.4872 (2)	0.6144 (3)	0.4348 (6)	0.0275 (10)
H12	0.5309	0.6369	0.4048	0.033*
C13	0.4452 (3)	0.5618 (3)	0.3286 (6)	0.0289 (10)
H13	0.4584	0.5482	0.2258	0.035*
C14	0.3827 (2)	0.5293 (3)	0.3769 (5)	0.0231 (9)
H14	0.3525	0.4923	0.3056	0.028*
N21	0.34829 (17)	0.4171 (2)	0.7928 (4)	0.0150 (7)
N22	0.4465 (2)	0.4159 (2)	1.0257 (5)	0.0285 (9)
C21	0.3925 (2)	0.4525 (3)	0.9200 (5)	0.0216 (9)
H21	0.3847	0.5093	0.9370	0.026*
C22	0.4557 (2)	0.3357 (3)	1.0026 (5)	0.0249 (9)
H22	0.4936	0.3074	1.0746	0.030*
C23	0.4125 (2)	0.2927 (3)	0.8790 (5)	0.0219 (9)
H23	0.4191	0.2354	0.8658	0.026*
C24	0.3587 (2)	0.3362 (2)	0.7736 (5)	0.0150 (8)
H24	0.3284	0.3080	0.6859	0.018*
N31	0.19048 (17)	0.5567 (2)	0.4101 (4)	0.0155 (7)
N32	0.09789 (17)	0.56059 (19)	0.1687 (4)	0.0143 (7)
C31	0.1369 (2)	0.5230 (2)	0.2998 (5)	0.0151 (8)
H31	0.1253	0.4670	0.3159	0.018*
C32	0.1156 (2)	0.6395 (2)	0.1491 (5)	0.0184 (8)
H32	0.0906	0.6684	0.0558	0.022*
C33	0.1689 (2)	0.6805 (3)	0.2591 (6)	0.0244 (9)
H33	0.1799	0.7368	0.2448	0.029*
C34	0.2051 (2)	0.6362 (2)	0.3899 (5)	0.0203 (9)
H34	0.2417	0.6627	0.4684	0.024*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Fe1	0.0097 (3)	0.0137 (3)	0.0102 (3)	−0.00061 (19)	0.0022 (2)	−0.0013 (2)
Fe2	0.0084 (3)	0.0124 (4)	0.0098 (4)	0.0004 (3)	0.0029 (3)	0.0014 (3)
N41	0.0200 (17)	0.0208 (18)	0.0212 (18)	−0.0004 (14)	0.0073 (15)	−0.0038 (14)
C41	0.0174 (18)	0.0167 (19)	0.020 (2)	0.0057 (15)	0.0032 (16)	−0.0026 (16)
S41	0.0447 (7)	0.0309 (7)	0.0414 (7)	0.0109 (5)	−0.0158 (6)	−0.0206 (6)
N51	0.0190 (17)	0.0198 (17)	0.0169 (17)	0.0001 (13)	0.0047 (14)	−0.0014 (14)
C51	0.0103 (16)	0.0106 (17)	0.0170 (19)	0.0005 (13)	0.0015 (14)	−0.0018 (14)
S51	0.0343 (6)	0.0272 (5)	0.0112 (5)	−0.0026 (4)	0.0052 (4)	−0.0027 (4)
N61	0.0162 (16)	0.0181 (17)	0.0161 (17)	0.0015 (12)	0.0035 (13)	0.0033 (13)
C61	0.0127 (17)	0.0131 (17)	0.0178 (19)	0.0037 (14)	0.0022 (15)	−0.0002 (15)
S61	0.0441 (7)	0.0281 (6)	0.0189 (5)	0.0067 (5)	0.0147 (5)	0.0085 (4)
N1	0.0085 (14)	0.0158 (16)	0.0155 (15)	−0.0002 (11)	0.0034 (12)	−0.0004 (12)
N2	0.0114 (14)	0.0153 (15)	0.0132 (15)	0.0004 (12)	0.0039 (12)	−0.0001 (12)
C1	0.0110 (16)	0.0159 (18)	0.0126 (17)	0.0012 (14)	0.0035 (14)	0.0007 (14)
C2	0.0151 (18)	0.0142 (18)	0.022 (2)	−0.0018 (14)	0.0075 (16)	0.0016 (15)
C3	0.0166 (18)	0.0114 (17)	0.026 (2)	−0.0026 (14)	0.0042 (16)	−0.0024 (15)
C4	0.0124 (17)	0.0175 (19)	0.020 (2)	0.0009 (14)	0.0039 (15)	−0.0038 (15)
N11	0.0107 (14)	0.0210 (17)	0.0153 (16)	−0.0021 (12)	0.0015 (13)	0.0017 (13)
N12	0.0231 (18)	0.032 (2)	0.027 (2)	−0.0136 (15)	0.0106 (16)	−0.0069 (16)
C11	0.0184 (19)	0.026 (2)	0.021 (2)	−0.0072 (16)	0.0072 (17)	−0.0056 (16)
C12	0.024 (2)	0.038 (3)	0.024 (2)	−0.0139 (19)	0.0140 (18)	−0.0027 (19)
C13	0.028 (2)	0.040 (3)	0.021 (2)	−0.012 (2)	0.0124 (19)	−0.0024 (19)
C14	0.024 (2)	0.031 (2)	0.015 (2)	−0.0097 (17)	0.0052 (17)	−0.0062 (17)
N21	0.0131 (15)	0.0181 (16)	0.0139 (15)	−0.0007 (12)	0.0026 (13)	0.0022 (13)
N22	0.0267 (19)	0.026 (2)	0.0274 (19)	−0.0014 (15)	−0.0108 (16)	0.0036 (16)
C21	0.025 (2)	0.021 (2)	0.0167 (19)	0.0001 (16)	−0.0026 (17)	0.0009 (16)
C22	0.021 (2)	0.027 (2)	0.026 (2)	0.0033 (17)	−0.0006 (18)	0.0084 (18)
C23	0.022 (2)	0.022 (2)	0.021 (2)	0.0063 (16)	0.0013 (17)	0.0055 (16)
C24	0.0157 (18)	0.0183 (19)	0.0114 (18)	0.0018 (14)	0.0036 (15)	0.0022 (14)
N31	0.0115 (15)	0.0181 (16)	0.0163 (16)	−0.0014 (12)	0.0011 (13)	0.0007 (13)
N32	0.0116 (15)	0.0154 (16)	0.0156 (16)	−0.0005 (12)	0.0012 (13)	−0.0015 (12)
C31	0.0112 (17)	0.0169 (18)	0.0165 (18)	0.0004 (14)	0.0010 (15)	−0.0004 (15)
C32	0.0155 (18)	0.0185 (19)	0.020 (2)	0.0003 (15)	−0.0008 (16)	0.0061 (15)
C33	0.023 (2)	0.017 (2)	0.031 (2)	−0.0046 (16)	−0.0027 (18)	0.0032 (17)
C34	0.0185 (19)	0.020 (2)	0.020 (2)	−0.0045 (15)	−0.0032 (16)	−0.0030 (16)

Fe1—N41	2.075 (3)	N12—C11	1.334 (5)
Fe1—N51	2.089 (3)	N12—C12	1.344 (6)
Fe1—N1	2.252 (3)	C11—H11	0.9500
Fe1—N31	2.254 (3)	C12—C13	1.364 (6)
Fe1—N21	2.262 (3)	C12—H12	0.9500
Fe1—N11	2.304 (3)	C13—C14	1.378 (6)
Fe2—N61	2.075 (3)	C13—H13	0.9500
Fe2—N61ⁱ	2.075 (3)	C14—H14	0.9500
Fe2—N2	2.252 (3)	N21—C21	1.340 (5)
Fe2—N2ⁱ	2.252 (3)	N21—C24	1.345 (5)
Fe2—N32ⁱⁱ	2.291 (3)	N22—C22	1.334 (6)
Fe2—N32ⁱⁱⁱ	2.291 (3)	N22—C21	1.339 (5)
N41—C41	1.161 (5)	C21—H21	0.9500
C41—S41	1.621 (4)	C22—C23	1.371 (6)
N51—C51	1.171 (5)	C22—H22	0.9500
C51—S51	1.619 (4)	C23—C24	1.388 (5)
N61—C61	1.169 (5)	C23—H23	0.9500
C61—S61	1.618 (4)	C24—H24	0.9500
N1—C1	1.341 (5)	N31—C31	1.335 (5)
N1—C4	1.344 (5)	N31—C34	1.338 (5)
N2—C1	1.335 (5)	N32—C31	1.338 (5)
N2—C2	1.343 (5)	N32—C32	1.343 (5)
C1—H1	0.9500	N32—Fe2^iv	2.291 (3)
C2—C3	1.380 (6)	C31—H31	0.9500
C2—H2	0.9500	C32—C33	1.382 (6)
C3—C4	1.379 (6)	C32—H32	0.9500
C3—H3	0.9500	C33—C34	1.372 (6)
C4—H4	0.9500	C33—H33	0.9500
N11—C14	1.336 (5)	C34—H34	0.9500
N11—C11	1.342 (5)

N41—Fe1—N51	178.69 (13)	N1—C4—H4	118.9
N41—Fe1—N1	90.82 (13)	C3—C4—H4	118.9
N51—Fe1—N1	88.50 (12)	C14—N11—C11	116.2 (3)
N41—Fe1—N31	91.24 (13)	C14—N11—Fe1	122.3 (3)
N51—Fe1—N31	87.72 (12)	C11—N11—Fe1	121.4 (3)
N1—Fe1—N31	96.10 (11)	C11—N12—C12	115.4 (4)
N41—Fe1—N21	92.26 (13)	N12—C11—N11	126.3 (4)
N51—Fe1—N21	88.85 (12)	N12—C11—H11	116.8
N1—Fe1—N21	89.70 (11)	N11—C11—H11	116.8
N31—Fe1—N21	173.18 (12)	N12—C12—C13	123.0 (4)
N41—Fe1—N11	90.18 (13)	N12—C12—H12	118.5
N51—Fe1—N11	90.56 (13)	C13—C12—H12	118.5
N1—Fe1—N11	176.83 (11)	C12—C13—C14	117.1 (4)
N31—Fe1—N11	86.88 (11)	C12—C13—H13	121.5
N21—Fe1—N11	87.25 (11)	C14—C13—H13	121.5
N61—Fe2—N61ⁱ	180.000 (1)	N11—C14—C13	122.0 (4)
N61—Fe2—N2	89.96 (12)	N11—C14—H14	119.0
N61ⁱ—Fe2—N2	90.04 (12)	C13—C14—H14	119.0
N61—Fe2—N2ⁱ	90.04 (12)	C21—N21—C24	115.9 (3)
N61ⁱ—Fe2—N2ⁱ	89.96 (12)	C21—N21—Fe1	123.5 (3)
N2—Fe2—N2ⁱ	180.000 (1)	C24—N21—Fe1	120.6 (2)
N61—Fe2—N32ⁱⁱ	90.10 (12)	C22—N22—C21	116.0 (4)
N61ⁱ—Fe2—N32ⁱⁱ	89.90 (12)	N22—C21—N21	126.6 (4)
N2—Fe2—N32ⁱⁱ	89.27 (11)	N22—C21—H21	116.7
N2ⁱ—Fe2—N32ⁱⁱ	90.73 (11)	N21—C21—H21	116.7
N61—Fe2—N32ⁱⁱⁱ	89.90 (12)	N22—C22—C23	122.4 (4)
N61ⁱ—Fe2—N32ⁱⁱⁱ	90.10 (12)	N22—C22—H22	118.8
N2—Fe2—N32ⁱⁱⁱ	90.73 (11)	C23—C22—H22	118.8
N2ⁱ—Fe2—N32ⁱⁱⁱ	89.27 (11)	C22—C23—C24	117.4 (4)
N32ⁱⁱ—Fe2—N32ⁱⁱⁱ	180.000 (1)	C22—C23—H23	121.3
C41—N41—Fe1	154.5 (3)	C24—C23—H23	121.3
N41—C41—S41	177.0 (4)	N21—C24—C23	121.6 (4)
C51—N51—Fe1	146.5 (3)	N21—C24—H24	119.2
N51—C51—S51	177.7 (3)	C23—C24—H24	119.2
C61—N61—Fe2	153.7 (3)	C31—N31—C34	116.8 (3)
N61—C61—S61	179.3 (4)	C31—N31—Fe1	124.8 (3)
C1—N1—C4	116.2 (3)	C34—N31—Fe1	118.2 (2)
C1—N1—Fe1	121.5 (2)	C31—N32—C32	115.6 (3)
C4—N1—Fe1	121.5 (3)	C31—N32—Fe2^iv	123.0 (3)
C1—N2—C2	116.5 (3)	C32—N32—Fe2^iv	121.2 (2)
C1—N2—Fe2	122.4 (2)	N31—C31—N32	126.1 (4)
C2—N2—Fe2	120.9 (3)	N31—C31—H31	117.0
N2—C1—N1	125.9 (3)	N32—C31—H31	117.0
N2—C1—H1	117.1	N32—C32—C33	122.7 (4)
N1—C1—H1	117.1	N32—C32—H32	118.7
N2—C2—C3	122.1 (4)	C33—C32—H32	118.7
N2—C2—H2	119.0	C34—C33—C32	116.9 (4)
C3—C2—H2	119.0	C34—C33—H33	121.6
C4—C3—C2	117.0 (4)	C32—C33—H33	121.6
C4—C3—H3	121.5	N31—C34—C33	121.9 (4)
C2—C3—H3	121.5	N31—C34—H34	119.0
N1—C4—C3	122.2 (4)	C33—C34—H34	119.0

Table 1

Selected bond lengths (Å)

Fe1—N41	2.075 (3)
Fe1—N51	2.089 (3)
Fe1—N1	2.252 (3)
Fe1—N31	2.254 (3)
Fe1—N21	2.262 (3)
Fe1—N11	2.304 (3)
Fe2—N61	2.075 (3)
Fe2—N61ⁱ	2.075 (3)
Fe2—N2	2.252 (3)
Fe2—N2ⁱ	2.252 (3)
Fe2—N32ⁱⁱ	2.291 (3)
Fe2—N32ⁱⁱⁱ	2.291 (3)

Symmetry codes: (i) ; (ii) ; (iii) .

2 in total

1. A short history of SHELX.

Authors: George M Sheldrick
Journal: Acta Crystallogr A Date: 2007-12-21 Impact factor: 2.290

2. Dimorphism of a new CuI coordination polymer:synthesis, crystal structures and properties of catena[CuI(2-iodopyrazine-N)] and poly[CuI(mu2-2-iodopyrazine-N,N')].

Authors: Christian Näther; Mario Wriedt; Inke Jess
Journal: Inorg Chem Date: 2003-04-07 Impact factor: 5.165

2 in total