Diiodidobis(4-methyl­pyridine N-oxide-κO)zinc(II)

The title mononuclear complex, [Zn(I)₂(C₆H₇NO)₂], lies on a special position of site symmetry 2. The Zn atom is coordinated by two I and two O atoms in a tetra­hedral geometry. There is a π–π stacking inter­action of the 4-methyl­pyridine N-oxide units.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.030
• wR factor = 0.075
• Data-to-parameter ratio = 18.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  I1     -   Zn1     ..       6.61 su
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         O1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C3

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2001); software used to prepare material for publication: SHELXTL.

Diiodidobis(4-methylpyridine N-oxide-?O)zinc(II)

Crystal data

[Zn(I)2(C6H7NO)2]	F(000) = 1008
Mr = 537.42	Dx = 2.052 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1828 reflections
a = 19.385 (5) Å	θ = 2.6–26.0°
b = 7.5134 (19) Å	µ = 4.96 mm^−1
c = 14.859 (4) Å	T = 293 K
β = 126.487 (3)°	Prism, colourless
V = 1739.9 (8) Å^3	0.21 × 0.12 × 0.09 mm
Z = 4

Data collection

Bruker SMART area-detector diffractometer	1597 independent reflections
Radiation source: fine-focus sealed tube	1371 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.029
φ and ω scans	θmax = 25.5°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −23→20
Tmin = 0.406, Tmax = 0.637	k = −9→8
4279 measured reflections	l = −17→17

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)] = 0.030	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.075	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.037P)^2] where P = (Fo^2 + 2Fc^2)/3
1597 reflections	(Δ/σ)max = 0.001
88 parameters	Δρmax = 0.59 e Å^−3
0 restraints	Δρmin = −0.49 e Å^−3

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

	x	y	z	Uiso*/Ueq
Zn1	0.5000	0.07038 (9)	0.7500	0.0502 (2)
N1	0.4751 (2)	0.2916 (4)	0.5765 (3)	0.0526 (8)
C1	0.4079 (3)	0.3817 (6)	0.5543 (5)	0.0653 (13)
H1	0.4025	0.4063	0.6112	0.078*
C2	0.3469 (3)	0.4381 (6)	0.4481 (5)	0.0690 (13)
H2	0.2999	0.5012	0.4333	0.083*
C3	0.3530 (3)	0.4039 (6)	0.3614 (4)	0.0617 (12)
C4	0.2878 (4)	0.4701 (8)	0.2442 (5)	0.1016 (19)
H4A	0.3054	0.5839	0.2351	0.152*
H4B	0.2331	0.4814	0.2308	0.152*
H4C	0.2832	0.3871	0.1917	0.152*
C5	0.4247 (3)	0.3109 (6)	0.3897 (4)	0.0626 (12)
H5	0.4324	0.2859	0.3349	0.075*
C6	0.4845 (3)	0.2552 (5)	0.4968 (4)	0.0556 (11)
H6	0.5322	0.1915	0.5143	0.067*
O1	0.53714 (19)	0.2360 (4)	0.6817 (3)	0.0680 (9)
I1	0.368720 (18)	−0.09837 (4)	0.59359 (3)	0.06272 (15)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0462 (4)	0.0652 (4)	0.0380 (4)	0.000	0.0244 (3)	0.000
N1	0.052 (2)	0.060 (2)	0.047 (2)	−0.0055 (18)	0.0300 (18)	0.0034 (18)
C1	0.068 (3)	0.079 (3)	0.063 (3)	0.005 (3)	0.047 (3)	0.000 (3)
C2	0.057 (3)	0.074 (3)	0.080 (4)	0.017 (2)	0.043 (3)	0.005 (3)
C3	0.060 (3)	0.060 (3)	0.053 (3)	0.000 (2)	0.027 (2)	0.003 (2)
C4	0.086 (4)	0.103 (4)	0.071 (4)	0.018 (4)	0.022 (3)	0.017 (4)
C5	0.072 (3)	0.071 (3)	0.051 (3)	0.005 (3)	0.040 (3)	−0.004 (2)
C6	0.057 (3)	0.061 (3)	0.056 (3)	0.011 (2)	0.038 (2)	0.007 (2)
O1	0.0528 (18)	0.093 (2)	0.0476 (18)	−0.0099 (17)	0.0241 (15)	0.0148 (17)
I1	0.0448 (2)	0.0832 (3)	0.0528 (2)	−0.00856 (14)	0.02497 (17)	−0.01277 (15)

Geometric parameters (Å, º)

Zn1—O1	1.992 (3)	C2—H2	0.9300
Zn1—O1^i	1.992 (3)	C3—C5	1.379 (7)
Zn1—I1	2.5399 (6)	C3—C4	1.503 (8)
Zn1—I1^i	2.5399 (6)	C4—H4A	0.9600
N1—C1	1.324 (6)	C4—H4B	0.9600
N1—C6	1.329 (5)	C4—H4C	0.9600
N1—O1	1.353 (4)	C5—C6	1.363 (6)
C1—C2	1.360 (7)	C5—H5	0.9300
C1—H1	0.9300	C6—H6	0.9300
C2—C3	1.387 (7)
O1—Zn1—O1^i	102.7 (2)	C5—C3—C4	121.4 (5)
O1—Zn1—I1	108.34 (9)	C2—C3—C4	122.5 (5)
O1^i—Zn1—I1	108.00 (9)	C3—C4—H4A	109.5
O1—Zn1—I1^i	108.00 (9)	C3—C4—H4B	109.5
O1^i—Zn1—I1^i	108.34 (9)	H4A—C4—H4B	109.5
I1—Zn1—I1^i	120.11 (3)	C3—C4—H4C	109.5
C1—N1—C6	121.3 (4)	H4A—C4—H4C	109.5
C1—N1—O1	120.8 (4)	H4B—C4—H4C	109.5
C6—N1—O1	117.8 (4)	C6—C5—C3	121.0 (4)
N1—C1—C2	119.8 (5)	C6—C5—H5	119.5
N1—C1—H1	120.1	C3—C5—H5	119.5
C2—C1—H1	120.1	N1—C6—C5	120.3 (4)
C1—C2—C3	121.6 (5)	N1—C6—H6	119.8
C1—C2—H2	119.2	C5—C6—H6	119.8
C3—C2—H2	119.2	N1—O1—Zn1	116.1 (2)
C5—C3—C2	116.0 (5)
C6—N1—C1—C2	0.2 (7)	O1—N1—C6—C5	−178.8 (4)
O1—N1—C1—C2	179.2 (4)	C3—C5—C6—N1	−0.8 (7)
N1—C1—C2—C3	−0.1 (8)	C1—N1—O1—Zn1	60.5 (4)
C1—C2—C3—C5	−0.5 (7)	C6—N1—O1—Zn1	−120.5 (3)
C1—C2—C3—C4	−177.9 (5)	O1^i—Zn1—O1—N1	−87.2 (3)
C2—C3—C5—C6	0.9 (7)	I1—Zn1—O1—N1	26.9 (3)
C4—C3—C5—C6	178.4 (5)	I1^i—Zn1—O1—N1	158.5 (2)
C1—N1—C6—C5	0.2 (7)

Symmetry code: (i) −x+1, y, −z+3/2.