The 1:2 adduct of hexa­aqua­nickel(II) dinitrate and bis­(pyrimidin-2-ylsulfan­yl)methane

In the title compound, hexa­aqua­nickel(II) dinitrate–bis­(pyrimidin-2-ylsulfan­yl)methane (1/2), [Ni(H₂O)₆](NO₃)₂·2C₉H₈N₄S₂, the Ni^II ion, located on an inversion center, has a distorted octa­hedral coordination geometry. The Ni^II complex cation, nitrate anions and the bis­(pyrimidin-2-ylsulf­an­yl)methane mol­ecules are linked together by hydrogen-bonding inter­actions.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.023
• wR factor = 0.068
• Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT233_ALERT_4_B Hirshfeld (M-X Solvent)    Ni1    -   OW2     ..      24.83 su
PLAT233_ALERT_4_B Hirshfeld (M-X Solvent)    Ni1    -   OW3     ..      26.42 su

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT233_ALERT_4_C Hirshfeld (M-X Solvent)    Ni1    -   OW1     ..      13.80 su
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          9

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

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

   3 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
   4 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: CrystalStructure (Rigaku, 2004).

hexaaquanickel(II) dinitrate–bis(pyrimidin-2-ylsulfanyl)methane (1/2)

Crystal data

[Ni(H2O)6](NO3)2·2C9H8N4S2	F(000) = 788
Mr = 763.45	Dx = 1.665 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9648 reflections
a = 14.078 (3) Å	θ = 3.0–27.5°
b = 8.0546 (16) Å	µ = 0.99 mm^−1
c = 14.887 (3) Å	T = 293 K
β = 115.56 (3)°	Block, light green
V = 1522.9 (7) Å^3	0.29 × 0.25 × 0.19 mm
Z = 2

Data collection

Rigaku R-AXIS RAPID IP area-detector diffractometer	2827 independent reflections
Radiation source: fine-focus sealed tube	2616 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.028
ω scans	θmax = 25.5°, θmin = 3.0°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −17→17
Tmin = 0.760, Tmax = 0.835	k = −9→9
11964 measured reflections	l = −17→18

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)] = 0.023	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.068	H-atom parameters constrained
S = 1.09	w = 1/[σ^2(Fo^2) + (0.0412P)^2 + 0.2626P] where P = (Fo^2 + 2Fc^2)/3
2827 reflections	(Δ/σ)max = 0.001
205 parameters	Δρmax = 0.22 e Å^−3
0 restraints	Δρmin = −0.30 e Å^−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
Ni1	1.0000	0.5000	0.5000	0.01410 (9)
S1	0.37682 (3)	0.56781 (5)	0.18042 (2)	0.02251 (11)
S2	0.61554 (3)	0.54918 (5)	0.31648 (2)	0.02212 (11)
OW1	0.88448 (8)	0.66073 (12)	0.45627 (7)	0.0224 (2)
HW1B	0.8432	0.6684	0.3927	0.034*
HW1A	0.8960	0.7673	0.4770	0.034*
OW2	0.98814 (10)	0.48238 (13)	0.35400 (8)	0.0315 (3)
HW2B	1.0079	0.3862	0.3409	0.047*
HW2A	1.0092	0.5481	0.3229	0.047*
OW3	0.88405 (8)	0.30222 (13)	0.45536 (7)	0.0284 (2)
HW3B	0.8998	0.2085	0.4813	0.043*
HW3A	0.8430	0.2826	0.3965	0.043*
N1	0.25487 (9)	0.70786 (16)	0.24938 (9)	0.0251 (3)
N2	0.40890 (10)	0.57822 (17)	0.37118 (9)	0.0268 (3)
N3	0.58548 (9)	0.57873 (17)	0.12676 (9)	0.0261 (3)
N4	0.74412 (9)	0.68548 (15)	0.25479 (9)	0.0228 (3)
C1	0.22617 (11)	0.7476 (2)	0.32125 (11)	0.0310 (4)
H1B	0.1641	0.8068	0.3044	0.037*
C2	0.28532 (13)	0.7041 (2)	0.41974 (12)	0.0339 (4)
H2B	0.2638	0.7304	0.4690	0.041*
C3	0.37731 (13)	0.6202 (2)	0.44108 (11)	0.0326 (4)
H3B	0.4196	0.5913	0.5069	0.039*
C4	0.34474 (10)	0.62239 (17)	0.27864 (10)	0.0205 (3)
C5	0.49296 (10)	0.44316 (18)	0.24598 (10)	0.0228 (3)
H5A	0.4794	0.3708	0.2912	0.027*
H5B	0.5024	0.3727	0.1976	0.027*
C6	0.65076 (10)	0.60945 (17)	0.22131 (10)	0.0197 (3)
C7	0.61878 (12)	0.6306 (2)	0.05956 (11)	0.0317 (4)
H7A	0.5763	0.6104	−0.0075	0.038*
C8	0.71243 (12)	0.7119 (2)	0.08497 (12)	0.0313 (4)
H8A	0.7336	0.7482	0.0371	0.038*
C9	0.77384 (11)	0.7372 (2)	0.18565 (11)	0.0284 (3)
H9A	0.8379	0.7920	0.2057	0.034*
O1	0.99396 (9)	1.12759 (13)	0.66059 (8)	0.0337 (3)
O2	0.91101 (11)	0.97077 (13)	0.53349 (9)	0.0381 (3)
O3	0.99144 (9)	0.86168 (13)	0.68037 (8)	0.0320 (3)
N5	0.96652 (10)	0.98701 (14)	0.62543 (10)	0.0227 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.01675 (14)	0.01332 (15)	0.01002 (14)	0.00164 (8)	0.00370 (10)	−0.00138 (8)
S1	0.02288 (19)	0.0266 (2)	0.01847 (19)	0.00013 (14)	0.00933 (15)	0.00006 (14)
S2	0.02318 (19)	0.0251 (2)	0.01765 (19)	0.00050 (14)	0.00842 (15)	0.00014 (14)
OW1	0.0243 (5)	0.0208 (5)	0.0174 (5)	0.0023 (4)	0.0046 (4)	−0.0029 (4)
OW2	0.0434 (7)	0.0240 (6)	0.0263 (6)	0.0001 (5)	0.0143 (5)	−0.0010 (4)
OW3	0.0342 (6)	0.0264 (6)	0.0192 (5)	0.0024 (4)	0.0065 (4)	0.0032 (4)
N1	0.0203 (6)	0.0301 (7)	0.0236 (6)	0.0004 (5)	0.0082 (5)	−0.0008 (5)
N2	0.0259 (6)	0.0348 (7)	0.0205 (6)	0.0035 (5)	0.0108 (5)	0.0045 (5)
N3	0.0224 (6)	0.0364 (7)	0.0184 (6)	−0.0025 (5)	0.0077 (5)	−0.0041 (5)
N4	0.0183 (6)	0.0261 (7)	0.0217 (6)	0.0015 (5)	0.0065 (5)	−0.0014 (5)
C1	0.0235 (7)	0.0401 (9)	0.0301 (8)	0.0014 (7)	0.0123 (6)	−0.0058 (7)
C2	0.0318 (8)	0.0470 (10)	0.0280 (8)	−0.0007 (7)	0.0177 (7)	−0.0054 (7)
C3	0.0329 (8)	0.0446 (10)	0.0207 (7)	0.0019 (8)	0.0120 (6)	0.0032 (7)
C4	0.0198 (6)	0.0218 (7)	0.0208 (7)	−0.0039 (6)	0.0098 (5)	−0.0006 (6)
C5	0.0249 (7)	0.0191 (8)	0.0264 (8)	−0.0006 (6)	0.0131 (6)	0.0003 (6)
C6	0.0191 (6)	0.0209 (7)	0.0184 (6)	0.0036 (5)	0.0073 (5)	−0.0007 (6)
C7	0.0284 (8)	0.0477 (10)	0.0180 (7)	0.0002 (7)	0.0091 (6)	−0.0018 (7)
C8	0.0286 (8)	0.0421 (9)	0.0272 (8)	0.0020 (7)	0.0159 (7)	0.0038 (7)
C9	0.0217 (7)	0.0331 (8)	0.0310 (8)	−0.0001 (6)	0.0118 (6)	−0.0003 (7)
O1	0.0431 (6)	0.0193 (6)	0.0348 (6)	−0.0086 (5)	0.0132 (5)	−0.0060 (5)
O2	0.0544 (8)	0.0254 (6)	0.0227 (6)	0.0012 (5)	0.0056 (5)	−0.0024 (5)
O3	0.0451 (7)	0.0209 (5)	0.0288 (6)	0.0054 (5)	0.0148 (5)	0.0049 (5)
N5	0.0251 (6)	0.0185 (6)	0.0264 (7)	−0.0004 (5)	0.0128 (5)	−0.0014 (5)

Geometric parameters (Å, º)

Ni1—OW1^i	1.9573 (10)	N3—C6	1.3308 (18)
Ni1—OW1	1.9573 (10)	N3—C7	1.342 (2)
Ni1—OW2^i	2.1116 (12)	N4—C9	1.334 (2)
Ni1—OW2	2.1116 (12)	N4—C6	1.3363 (18)
Ni1—OW3	2.1698 (11)	C1—C2	1.383 (2)
Ni1—OW3^i	2.1698 (11)	C1—H1B	0.9300
S1—C4	1.7621 (14)	C2—C3	1.371 (2)
S1—C5	1.8047 (15)	C2—H2B	0.9300
S2—C6	1.7592 (14)	C3—H3B	0.9300
S2—C5	1.8017 (15)	C5—H5A	0.9700
OW1—HW1B	0.8731	C5—H5B	0.9700
OW1—HW1A	0.9030	C7—C8	1.371 (2)
OW2—HW2B	0.8729	C7—H7A	0.9300
OW2—HW2A	0.8372	C8—C9	1.385 (2)
OW3—HW3B	0.8336	C8—H8A	0.9300
OW3—HW3A	0.8299	C9—H9A	0.9300
N1—C1	1.335 (2)	O1—N5	1.2373 (16)
N1—C4	1.3376 (19)	O2—N5	1.2564 (18)
N2—C4	1.3291 (19)	O3—N5	1.2504 (16)
N2—C3	1.340 (2)
OW1^i—Ni1—OW1	180.0	C2—C1—H1B	118.8
OW1^i—Ni1—OW2^i	90.96 (5)	C3—C2—C1	116.55 (15)
OW1—Ni1—OW2^i	89.04 (5)	C3—C2—H2B	121.7
OW1^i—Ni1—OW2	89.04 (5)	C1—C2—H2B	121.7
OW1—Ni1—OW2	90.96 (5)	N2—C3—C2	122.78 (14)
OW2^i—Ni1—OW2	180.0	N2—C3—H3B	118.6
OW1^i—Ni1—OW3	91.35 (5)	C2—C3—H3B	118.6
OW1—Ni1—OW3	88.65 (5)	N2—C4—N1	126.85 (13)
OW2^i—Ni1—OW3	94.57 (5)	N2—C4—S1	119.37 (11)
OW2—Ni1—OW3	85.43 (5)	N1—C4—S1	113.78 (10)
OW1^i—Ni1—OW3^i	88.65 (5)	S2—C5—S1	117.90 (8)
OW1—Ni1—OW3^i	91.35 (5)	S2—C5—H5A	107.8
OW2^i—Ni1—OW3^i	85.43 (5)	S1—C5—H5A	107.8
OW2—Ni1—OW3^i	94.57 (5)	S2—C5—H5B	107.8
OW3—Ni1—OW3^i	180.00 (4)	S1—C5—H5B	107.8
C4—S1—C5	100.76 (7)	H5A—C5—H5B	107.2
C6—S2—C5	101.16 (7)	N3—C6—N4	126.81 (13)
Ni1—OW1—HW1B	118.5	N3—C6—S2	119.64 (11)
Ni1—OW1—HW1A	121.0	N4—C6—S2	113.55 (10)
HW1B—OW1—HW1A	103.9	N3—C7—C8	123.14 (14)
Ni1—OW2—HW2B	113.4	N3—C7—H7A	118.4
Ni1—OW2—HW2A	129.5	C8—C7—H7A	118.4
HW2B—OW2—HW2A	102.4	C7—C8—C9	116.48 (15)
Ni1—OW3—HW3B	120.5	C7—C8—H8A	121.8
Ni1—OW3—HW3A	123.5	C9—C8—H8A	121.8
HW3B—OW3—HW3A	104.0	N4—C9—C8	122.15 (14)
C1—N1—C4	115.67 (13)	N4—C9—H9A	118.9
C4—N2—C3	115.63 (13)	C8—C9—H9A	118.9
C6—N3—C7	115.26 (13)	O1—N5—O3	120.92 (13)
C9—N4—C6	116.15 (12)	O1—N5—O2	119.35 (12)
N1—C1—C2	122.46 (14)	O3—N5—O2	119.72 (12)
N1—C1—H1B	118.8
C4—N1—C1—C2	0.2 (2)	C4—S1—C5—S2	−79.04 (9)
N1—C1—C2—C3	1.4 (3)	C7—N3—C6—N4	0.1 (2)
C4—N2—C3—C2	−0.4 (2)	C7—N3—C6—S2	179.43 (11)
C1—C2—C3—N2	−1.3 (3)	C9—N4—C6—N3	0.8 (2)
C3—N2—C4—N1	2.2 (2)	C9—N4—C6—S2	−178.60 (11)
C3—N2—C4—S1	−178.13 (11)	C5—S2—C6—N3	3.79 (13)
C1—N1—C4—N2	−2.2 (2)	C5—S2—C6—N4	−176.78 (10)
C1—N1—C4—S1	178.19 (11)	C6—N3—C7—C8	−1.0 (2)
C5—S1—C4—N2	4.87 (13)	N3—C7—C8—C9	0.9 (3)
C5—S1—C4—N1	−175.46 (10)	C6—N4—C9—C8	−0.8 (2)
C6—S2—C5—S1	−78.34 (9)	C7—C8—C9—N4	0.0 (2)

Symmetry code: (i) −x+2, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
OW1—HW1A···O2	0.90	1.81	2.7068 (15)	170
OW1—HW1B···N4	0.87	1.93	2.7977 (19)	176
OW2—HW2A···O3^ii	0.84	2.15	2.8922 (17)	147
OW2—HW2B···O3^i	0.87	2.02	2.8550 (16)	159
OW3—HW3A···N1^iii	0.83	2.10	2.9239 (19)	174
OW3—HW3B···O2^iv	0.83	2.05	2.8711 (16)	170
C1—H1B···O1^v	0.93	2.55	3.378 (2)	149
C9—H9A···O1^vi	0.93	2.43	3.264 (2)	149

Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) x, −y+3/2, z−1/2; (iii) −x+1, y−1/2, −z+1/2; (iv) x, y−1, z; (v) −x+1, −y+2, −z+1; (vi) −x+2, −y+2, −z+1.