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In the title complex, [Ni(NCS)2(H2O)4]·4C6H9N3·2H2O, the nickel(II) ion occupies an inversion centre and is octahedrally coordinated by two N-bonded thio­cyanate ions and four water mol­ecules. The two distinct 2-amino-4,6-di­methyl­pyrimidine mol­ecules adopt distinct base-pairing dimerization patterns via different pairs of N—H...N bonds. They are also hydrogen bonded to the coordinated and uncoordinated water mol­ecules and thio­cyanate ions through O—H...O, O—H...S(thio­cyanate) and N—H...N(thio­cyanate) hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804033884/hb6132sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804033884/hb6132Isup2.hkl
Contains datablock I

CCDC reference: 254309

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.045
  • wR factor = 0.115
  • Data-to-parameter ratio = 20.3

checkCIF/PLATON results

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Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.66 mm PLAT230_ALERT_2_C Hirshfeld Test Diff for S1 - C7 .. 6.78 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni - N4 .. 5.18 su PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2A ... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 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 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker 2001); cell refinement: SMART; data reduction: SHELXTL (Bruker 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON.

Tetraaquadithiocyanatonickel(II) tetrakis(2-amino-4,6-dimethylpyrimidine) dihydrate top
Crystal data top
[Ni(C6H8N2O4S2)]·4C6H9N3·2H2OZ = 1
Mr = 775.61F(000) = 410
Triclinic, P1Dx = 1.339 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.8006 (5) ÅCell parameters from 7595 reflections
b = 11.6289 (8) Åθ = 1.9–28.3°
c = 11.9121 (8) ŵ = 0.67 mm1
α = 67.701 (1)°T = 293 K
β = 75.488 (1)°Plate, pale green
γ = 78.896 (1)°0.66 × 0.60 × 0.15 mm
V = 962.12 (11) Å3
Data collection top
Bruker SMART CCD
diffractometer
4605 independent reflections
Radiation source: fine-focus sealed tube3465 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ω scansθmax = 28.3°, θmin = 1.9°
Absorption correction: part of the refinement model (ΔF)
(SHELXA; Bruker, 2001)
h = 1010
Tmin = 0.667, Tmax = 0.906k = 1415
7595 measured reflectionsl = 1514
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.045Hydrogen site location: difmap (O-H) and geom (others)
wR(F2) = 0.115H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0548P)2 + 0.1851P]
where P = (Fo2 + 2Fc2)/3
4605 reflections(Δ/σ)max < 0.001
227 parametersΔρmax = 0.23 e Å3
9 restraintsΔρmin = 0.25 e Å3
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Refinement. Refinement on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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 (Å2) top
xyzUiso*/Ueq
Ni0.500000.000000.500000.0370 (1)
S10.18407 (10)0.34064 (7)0.21736 (7)0.0641 (3)
O10.6856 (2)0.10938 (15)0.49346 (14)0.0487 (6)
O20.3409 (2)0.02895 (15)0.65679 (14)0.0488 (5)
N40.3736 (3)0.15530 (19)0.38445 (19)0.0512 (7)
C70.2957 (3)0.2330 (2)0.3146 (2)0.0430 (7)
N10.6246 (2)0.14024 (16)0.90636 (16)0.0389 (5)
N20.6038 (3)0.01818 (18)0.84202 (17)0.0482 (7)
N30.7493 (3)0.14728 (18)0.69873 (16)0.0423 (6)
C10.6589 (3)0.0934 (2)0.81431 (19)0.0360 (6)
C20.8054 (3)0.2587 (2)0.6720 (2)0.0432 (7)
C30.7726 (3)0.3144 (2)0.7601 (2)0.0465 (8)
C40.6825 (3)0.2509 (2)0.8777 (2)0.0429 (7)
C50.6470 (4)0.3024 (3)0.9808 (3)0.0654 (10)
C60.9074 (4)0.3179 (3)0.5438 (2)0.0636 (10)
N1A0.2735 (2)0.24335 (15)0.71178 (16)0.0391 (6)
N2A0.4108 (3)0.35410 (18)0.51457 (18)0.0554 (7)
N3A0.3587 (3)0.44709 (16)0.65994 (17)0.0406 (6)
C1A0.3462 (3)0.34771 (19)0.63175 (19)0.0382 (6)
C2A0.2892 (3)0.4423 (2)0.7759 (2)0.0424 (7)
C3A0.2071 (3)0.3405 (2)0.8623 (2)0.0472 (8)
C4A0.2040 (3)0.2410 (2)0.82764 (19)0.0396 (6)
C5A0.1250 (4)0.1235 (2)0.9160 (2)0.0541 (8)
C6A0.3056 (4)0.5531 (3)0.8068 (3)0.0669 (11)
O31.0299 (3)0.0856 (2)0.6988 (2)0.0839 (9)
H110.707800.115700.561000.0590*
H120.794900.106000.442300.0590*
H210.236500.005300.680600.0590*
H220.309000.105000.669300.0590*
H2A0.626400.052700.786800.0580*
H2B0.545700.055200.915000.0580*
H30.809800.392100.741200.0560*
H5A0.710800.248201.044200.0980*
H5B0.521700.307601.014900.0980*
H5C0.686000.384200.949000.0980*
H6A1.013300.263800.528600.0950*
H6B0.939600.396600.535800.0950*
H6C0.834700.331100.484900.0950*
H21A0.457600.419600.461300.0660*
H22B0.405600.292700.492500.0660*
H31A0.155300.339300.942000.0570*
H51A0.036000.107300.882600.0810*
H52B0.071500.133600.994000.0810*
H53C0.217000.054500.927700.0810*
H61A0.264500.628500.746000.1000*
H62B0.428000.555000.806900.1000*
H63C0.234800.546700.887000.1000*
H310.925900.033800.709100.1010*
H320.992200.165400.747500.1010*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0433 (2)0.0385 (2)0.0349 (2)0.0090 (2)0.0065 (2)0.0176 (2)
S10.0690 (5)0.0602 (4)0.0543 (4)0.0009 (3)0.0201 (3)0.0081 (3)
O10.0520 (10)0.0619 (10)0.0448 (9)0.0203 (8)0.0024 (7)0.0300 (8)
O20.0541 (10)0.0511 (9)0.0485 (9)0.0166 (8)0.0037 (8)0.0288 (8)
N40.0577 (13)0.0488 (11)0.0510 (12)0.0061 (10)0.0146 (10)0.0191 (10)
C70.0489 (14)0.0448 (12)0.0397 (12)0.0107 (10)0.0027 (10)0.0207 (10)
N10.0435 (10)0.0434 (9)0.0334 (9)0.0051 (8)0.0063 (8)0.0181 (8)
N20.0637 (13)0.0507 (11)0.0363 (10)0.0206 (10)0.0007 (9)0.0216 (9)
N30.0441 (11)0.0557 (11)0.0328 (9)0.0158 (9)0.0028 (8)0.0197 (8)
C10.0330 (11)0.0450 (11)0.0332 (10)0.0062 (9)0.0058 (9)0.0166 (9)
C20.0393 (12)0.0541 (13)0.0374 (12)0.0106 (10)0.0083 (10)0.0141 (10)
C30.0528 (14)0.0423 (12)0.0484 (13)0.0114 (10)0.0122 (11)0.0159 (10)
C40.0440 (13)0.0466 (12)0.0448 (12)0.0024 (10)0.0101 (10)0.0237 (10)
C50.085 (2)0.0654 (16)0.0593 (17)0.0139 (15)0.0046 (15)0.0397 (14)
C60.0695 (19)0.0775 (18)0.0420 (14)0.0310 (15)0.0057 (13)0.0111 (13)
N1A0.0440 (11)0.0345 (9)0.0383 (10)0.0099 (8)0.0041 (8)0.0121 (7)
N2A0.0853 (16)0.0428 (10)0.0405 (11)0.0280 (11)0.0079 (10)0.0198 (9)
N3A0.0479 (11)0.0369 (9)0.0401 (10)0.0103 (8)0.0053 (8)0.0162 (8)
C1A0.0417 (12)0.0363 (10)0.0387 (11)0.0072 (9)0.0060 (9)0.0152 (9)
C2A0.0447 (13)0.0464 (12)0.0427 (12)0.0026 (10)0.0107 (10)0.0224 (10)
C3A0.0508 (14)0.0568 (14)0.0357 (12)0.0083 (11)0.0028 (10)0.0204 (10)
C4A0.0353 (11)0.0422 (11)0.0370 (11)0.0039 (9)0.0072 (9)0.0090 (9)
C5A0.0540 (15)0.0502 (13)0.0447 (13)0.0118 (12)0.0013 (11)0.0042 (11)
C6A0.086 (2)0.0649 (17)0.0660 (18)0.0158 (15)0.0081 (16)0.0413 (15)
O30.0488 (12)0.0948 (16)0.1185 (19)0.0208 (11)0.0125 (12)0.0606 (15)
Geometric parameters (Å, º) top
Ni—O12.0731 (17)N3A—C2A1.335 (3)
Ni—O22.0728 (16)N2A—H22B0.8600
Ni—N42.058 (2)N2A—H21A0.8604
Ni—O1i2.0731 (17)C2—C31.380 (3)
Ni—O2i2.0728 (16)C2—C61.498 (3)
Ni—N4i2.058 (2)C3—C41.387 (3)
S1—C71.629 (2)C4—C51.506 (4)
O1—H110.8957C3—H30.9302
O1—H120.9191C5—H5C0.9598
O2—H210.9087C5—H5A0.9600
O2—H220.9289C5—H5B0.9596
O3—H320.9462C6—H6C0.9600
O3—H310.9241C6—H6B0.9592
N4—C71.162 (3)C6—H6A0.9604
N1—C41.338 (3)C2A—C6A1.503 (4)
N1—C11.349 (3)C2A—C3A1.381 (3)
N2—C11.340 (3)C3A—C4A1.374 (3)
N3—C21.344 (3)C4A—C5A1.504 (3)
N3—C11.347 (3)C3A—H31A0.9299
N2—H2B0.8603C5A—H52B0.9596
N2—H2A0.8602C5A—H53C0.9601
N1A—C1A1.349 (3)C5A—H51A0.9599
N1A—C4A1.342 (3)C6A—H63C0.9595
N2A—C1A1.338 (3)C6A—H61A0.9604
N3A—C1A1.346 (3)C6A—H62B0.9596
O1—Ni—O291.75 (6)N1—C4—C3122.1 (2)
O1—Ni—N489.45 (8)N1—C4—C5116.4 (2)
O1—Ni—O1i180.00C3—C4—C5121.5 (2)
O1—Ni—O2i88.25 (6)C2—C3—H3121.03
O1—Ni—N4i90.55 (8)C4—C3—H3121.05
O2—Ni—N492.20 (8)C4—C5—H5B109.45
O1i—Ni—O288.25 (6)C4—C5—H5A109.47
O2—Ni—O2i180.00H5A—C5—H5B109.50
O2—Ni—N4i87.80 (8)C4—C5—H5C109.47
O1i—Ni—N490.55 (8)H5B—C5—H5C109.51
O2i—Ni—N487.80 (8)H5A—C5—H5C109.43
N4—Ni—N4i180.00C2—C6—H6B109.46
O1i—Ni—O2i91.75 (6)C2—C6—H6C109.47
O1i—Ni—N4i89.45 (8)C2—C6—H6A109.44
O2i—Ni—N4i92.20 (8)H6A—C6—H6B109.47
Ni—O1—H12118.16H6B—C6—H6C109.50
H11—O1—H12105.38H6A—C6—H6C109.48
Ni—O1—H11123.29N1A—C1A—N3A125.24 (19)
H21—O2—H22103.87N2A—C1A—N3A116.9 (2)
Ni—O2—H21112.91N1A—C1A—N2A117.9 (2)
Ni—O2—H22126.32N3A—C2A—C3A121.4 (2)
H31—O3—H32101.61N3A—C2A—C6A116.4 (2)
Ni—N4—C7171.8 (2)C3A—C2A—C6A122.1 (2)
C1—N1—C4116.26 (18)C2A—C3A—C4A118.4 (2)
C1—N3—C2117.2 (2)N1A—C4A—C5A116.1 (2)
H2A—N2—H2B120.03C3A—C4A—C5A122.63 (19)
C1—N2—H2B119.98N1A—C4A—C3A121.3 (2)
C1—N2—H2A119.99C4A—C3A—H31A120.81
C1A—N1A—C4A116.75 (19)C2A—C3A—H31A120.81
C1A—N3A—C2A116.8 (2)C4A—C5A—H51A109.45
C1A—N2A—H22B119.99C4A—C5A—H52B109.51
C1A—N2A—H21A120.03H51A—C5A—H52B109.46
H21A—N2A—H22B119.97H51A—C5A—H53C109.39
S1—C7—N4179.1 (2)C4A—C5A—H53C109.51
N1—C1—N2116.96 (19)H52B—C5A—H53C109.51
N1—C1—N3125.4 (2)C2A—C6A—H62B109.45
N2—C1—N3117.6 (2)C2A—C6A—H63C109.55
N3—C2—C3121.1 (2)C2A—C6A—H61A109.41
C3—C2—C6121.8 (2)H61A—C6A—H63C109.46
N3—C2—C6117.1 (2)H62B—C6A—H63C109.51
C2—C3—C4117.9 (2)H61A—C6A—H62B109.44
O2—Ni—O1—H1131.49C2—N3—C1—N12.1 (4)
O2—Ni—O1—H12166.82C2—N3—C1—N2179.5 (2)
N4—Ni—O1—H11123.67C1—N3—C2—C30.6 (4)
N4—Ni—O1—H12100.99C1—N3—C2—C6179.4 (2)
O2i—Ni—O1—H11148.51C4A—N1A—C1A—N2A177.7 (2)
O2i—Ni—O1—H1213.18C4A—N1A—C1A—N3A2.0 (3)
N4i—Ni—O1—H1156.33C1A—N1A—C4A—C3A0.1 (3)
N4i—Ni—O1—H1279.01C1A—N1A—C4A—C5A179.5 (2)
O1—Ni—O2—H21175.29C1A—N3A—C2A—C3A0.5 (4)
O1—Ni—O2—H2245.96C1A—N3A—C2A—C6A179.4 (2)
N4—Ni—O2—H2185.77C2A—N3A—C1A—N1A1.7 (4)
N4—Ni—O2—H2243.55C2A—N3A—C1A—N2A178.0 (2)
O1i—Ni—O2—H214.71N3—C2—C3—C41.0 (4)
O1i—Ni—O2—H22134.04C6—C2—C3—C4177.8 (2)
N4i—Ni—O2—H2194.23C2—C3—C4—N11.4 (4)
N4i—Ni—O2—H22136.45C2—C3—C4—C5177.7 (2)
C4—N1—C1—N2179.1 (2)C6A—C2A—C3A—C4A177.5 (2)
C4—N1—C1—N31.7 (3)N3A—C2A—C3A—C4A2.4 (4)
C1—N1—C4—C30.1 (3)C2A—C3A—C4A—N1A2.1 (4)
C1—N1—C4—C5179.0 (2)C2A—C3A—C4A—C5A177.3 (2)
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2B···N1ii0.862.183.040 (3)175
O1—H11···N30.901.922.816 (3)174
O1—H12···O3iii0.921.942.818 (3)159
O2—H21···O3iv0.911.942.836 (3)168
N2A—H21A···N3Av0.862.162.997 (3)164
O2—H22···N1A0.931.822.736 (3)170
N2A—H22B···N40.862.483.322 (3)167
O3—H31···N30.922.263.137 (3)158
O3—H32···S1i0.952.523.377 (3)150
Symmetry codes: (i) x+1, y, z+1; (ii) x+1, y, z+2; (iii) x+2, y, z+1; (iv) x1, y, z; (v) x+1, y+1, z+1.
 

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