Tetra­aqua­bis(thio­cyanato-κN)zinc(II) bis­(2-methyl­pyrazine 1,4-dioxide)

In the title compound, [Zn(NCS)₂(H₂O)₄]·2C₅H₆N₂O₂, the six-coordinated Zn^II atom lies on a special position of site symmetry 2/m. The methyl­pyrazine dioxide mol­ecule lies on a mirror plane and links with the Zn^II complex via O—H...O hydrogen bonding.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.037
• wR factor = 0.099
• Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety         C5

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

   1 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
   0 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 (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 (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Tetraaquabis(isothiocyanato-κN)zinc(II) bis(2-methylpyrazine 1,4-dioxide)

Crystal data

[Zn(NCS)2(H2O)4]·2C5H6N2O2	F(000) = 520
Mr = 505.83	Dx = 1.551 Mg m^−3
Monoclinic, C2/m	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2y	Cell parameters from 2336 reflections
a = 16.985 (6) Å	θ = 2.2–27.0°
b = 6.775 (2) Å	µ = 1.38 mm^−1
c = 10.141 (3) Å	T = 298 K
β = 111.879 (4)°	Prism, colorless
V = 1082.9 (6) Å^3	0.22 × 0.12 × 0.08 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	1275 independent reflections
Radiation source: fine-focus sealed tube	1198 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.027
φ and ω scans	θmax = 27.0°, θmin = 2.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −21→15
Tmin = 0.752, Tmax = 0.898	k = −8→8
3156 measured reflections	l = −9→12

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)] = 0.037	H-atom parameters constrained
wR(F^2) = 0.099	w = 1/[σ^2(Fo^2) + (0.0576P)^2 + 0.4793P] where P = (Fo^2 + 2Fc^2)/3
S = 1.12	(Δ/σ)max = 0.001
1275 reflections	Δρmax = 0.51 e Å^−3
87 parameters	Δρmin = −0.84 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.032 (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
Zn1	0.5000	0.0000	1.0000	0.0351 (2)
S1	0.19557 (4)	0.0000	0.74267 (9)	0.0474 (3)
N1	0.37160 (17)	0.0000	0.8694 (3)	0.0488 (6)
O1	0.46979 (8)	0.2273 (2)	1.11800 (15)	0.0424 (4)
H1	0.4457	0.1863	1.1719	0.064*
H2	0.5090	0.3047	1.1654	0.064*
C5	0.3875 (2)	0.0000	0.5288 (4)	0.0725 (13)
H7	0.4199	0.0971	0.5328	0.109*
H6	0.3699	0.0000	0.6063	0.109*
C6	0.29833 (17)	0.0000	0.8167 (3)	0.0362 (6)
O2	0.40187 (12)	0.0000	0.2734 (2)	0.0457 (5)
N2	0.32504 (14)	0.0000	0.2719 (2)	0.0336 (5)
C4	0.25770 (18)	0.0000	0.1475 (3)	0.0410 (6)
H4	0.2667	0.0000	0.0625	0.049*
C1	0.31237 (17)	0.0000	0.3962 (3)	0.0380 (6)
O3	0.08688 (12)	0.0000	0.2678 (3)	0.0477 (5)
N3	0.16399 (12)	0.0000	0.2671 (2)	0.0349 (5)
C2	0.23054 (17)	0.0000	0.3912 (3)	0.0386 (6)
H5A	0.2210	0.0000	0.4757	0.046*
C3	0.17709 (18)	0.0000	0.1446 (3)	0.0413 (6)
H3	0.1313	0.0000	0.0582	0.050*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0295 (3)	0.0400 (3)	0.0345 (3)	0.000	0.01033 (19)	0.000
S1	0.0322 (4)	0.0462 (4)	0.0540 (5)	0.000	0.0048 (3)	0.000
N1	0.0372 (13)	0.0599 (16)	0.0430 (14)	0.000	0.0075 (11)	0.000
O1	0.0377 (7)	0.0478 (8)	0.0440 (8)	−0.0062 (6)	0.0179 (6)	−0.0066 (6)
C5	0.0348 (16)	0.139 (4)	0.0356 (17)	0.000	0.0032 (13)	0.000
C6	0.0384 (14)	0.0362 (13)	0.0312 (13)	0.000	0.0098 (11)	0.000
O2	0.0350 (10)	0.0568 (12)	0.0515 (12)	0.000	0.0232 (9)	0.000
N2	0.0307 (10)	0.0357 (11)	0.0343 (11)	0.000	0.0121 (9)	0.000
C4	0.0440 (14)	0.0476 (15)	0.0296 (13)	0.000	0.0118 (11)	0.000
C1	0.0312 (12)	0.0512 (15)	0.0297 (13)	0.000	0.0092 (10)	0.000
O3	0.0257 (9)	0.0527 (13)	0.0625 (13)	0.000	0.0138 (9)	0.000
N3	0.0245 (10)	0.0356 (11)	0.0403 (12)	0.000	0.0071 (9)	0.000
C2	0.0335 (13)	0.0494 (15)	0.0316 (13)	0.000	0.0108 (11)	0.000
C3	0.0371 (13)	0.0445 (15)	0.0316 (13)	0.000	0.0003 (10)	0.000

Geometric parameters (Å, º)

Zn1—N1^i	2.088 (3)	C5—H6	0.9388
Zn1—N1	2.088 (3)	O2—N2	1.299 (3)
Zn1—O1^i	2.1271 (14)	N2—C4	1.350 (4)
Zn1—O1	2.1271 (14)	N2—C1	1.356 (3)
Zn1—O1^ii	2.1271 (14)	C4—C3	1.358 (4)
Zn1—O1^iii	2.1271 (14)	C4—H4	0.9300
S1—C6	1.623 (3)	C1—C2	1.372 (4)
N1—C6	1.157 (4)	O3—N3	1.312 (3)
O1—H1	0.8420	N3—C3	1.341 (4)
O1—H2	0.8427	N3—C2	1.342 (3)
C5—C1	1.469 (4)	C2—H5A	0.9300
C5—H7	0.8491	C3—H3	0.9300
N1^i—Zn1—N1	180.00 (9)	H7—C5—H6	111.3
N1^i—Zn1—O1^i	86.74 (7)	N1—C6—S1	180.0 (3)
N1—Zn1—O1^i	93.26 (7)	O2—N2—C4	120.6 (2)
N1^i—Zn1—O1	93.26 (7)	O2—N2—C1	119.7 (2)
N1—Zn1—O1	86.74 (7)	C4—N2—C1	119.7 (2)
O1^i—Zn1—O1	180.0	N2—C4—C3	121.1 (3)
N1^i—Zn1—O1^ii	93.26 (7)	N2—C4—H4	119.4
N1—Zn1—O1^ii	86.74 (7)	C3—C4—H4	119.4
O1^i—Zn1—O1^ii	87.22 (8)	N2—C1—C2	118.4 (2)
O1—Zn1—O1^ii	92.78 (8)	N2—C1—C5	117.8 (2)
N1^i—Zn1—O1^iii	86.74 (7)	C2—C1—C5	123.8 (3)
N1—Zn1—O1^iii	93.26 (7)	O3—N3—C3	121.0 (2)
O1^i—Zn1—O1^iii	92.78 (8)	O3—N3—C2	119.2 (2)
O1—Zn1—O1^iii	87.22 (8)	C3—N3—C2	119.8 (2)
O1^ii—Zn1—O1^iii	180.000 (1)	N3—C2—C1	121.5 (2)
C6—N1—Zn1	169.3 (3)	N3—C2—H5A	119.3
Zn1—O1—H1	113.8	C1—C2—H5A	119.3
Zn1—O1—H2	117.8	N3—C3—C4	119.6 (2)
H1—O1—H2	107.8	N3—C3—H3	120.2
C1—C5—H7	111.7	C4—C3—H3	120.2
C1—C5—H6	109.2

Symmetry codes: (i) −x+1, −y, −z+2; (ii) x, −y, z; (iii) −x+1, y, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O2^iv	0.84	1.94	2.746 (2)	159
O1—H2···O3^v	0.84	1.89	2.725 (2)	173

Symmetry codes: (iv) x, y, z+1; (v) x+1/2, y+1/2, z+1.