Bis(5,8-diazo­niadispiro­[4.2.4.2]tetra­deca­ne) hexa­kis(thio­cyanato-κN)nickelate(II) dihydrate

Song, M.-P.; Li, L.-K.; Wu, B.-L.; Niu, Y.-Y.

doi:10.1107/S1600536807035416

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Bis(5,8-diazoniadispiro[4.2.4.2]tetradecane) hexakis(thiocyanato-κN)nickelate(II) dihydrate

M.-P. Song, L.-K. Li, B.-L. Wu and Y.-Y. Niu

The asymmetric unit of the title compound, (C₁₂H₂₄N₂)₂[Ni(NCS)₆]·2H₂O, comprises one cation, one half-anion and one water molecule. The anion lies on an inversion centre and shows the expected octahedral coordination with only minor deviations from the ideal geometry. Intermolecular O—H

S, O—H

N, C—H

S, C—H

O and C—H

N hydrogen-bonding interactions link all components into a three-dimensional extended network.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807035416/rz2160sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807035416/rz2160Isup2.hkl Contains datablock I

CCDC reference: 657630

checkCIF report

Key indicators

Single-crystal X-ray study
T = 273 K
Mean (C-C) = 0.004 Å
R factor = 0.038
wR factor = 0.105
Data-to-parameter ratio = 15.8

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT230_ALERT_2_C Hirshfeld Test Diff for    S1     -   C1      ..       5.74 su
PLAT230_ALERT_2_C Hirshfeld Test Diff for    S3     -   C3      ..       5.17 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Ni1    -   N2      ..       5.80 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Ni1    -   N3      ..       5.27 su
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C13
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C2
PLAT355_ALERT_3_C Long    O-H Bond (0.82A)   O1     -   H1C    ...       1.05 Ang.

Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni1         (2)       2.11

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

Comment top

Organo-inorganic hybrid compounds containing the hexakis(isothiocyanato)nickel(II) tetraanion have been the subject of several investigations, but the structural examples are scarce (Vicente et al., 1996; Kruger & McKee, 1996; Hoffman & Wood, 1982). In this work we present the crystal structure of a new hexakis(isothiocyanato)nickel(II) salt with the 5,8-diazoniadispiro[4.2.4.2]tetradecane dication.

The structure of the title compound (Fig. 1) comprises discrete (C₁₂H₂₄N₂)²⁺ cations, [Ni(NCS)₆]^4- anions and water molecules in the ratio 2:1:2. The anion, which lies on an inversion centre, displays the expected N⁶-octahedral coordination with only minor deviations from the ideal geometry. In the cation, the six-membered ring displays a chair conformation, while the five-membered rings adopt a twist conformation. In the crystal structure, all components are linked into a three-dimensional extended network through intermolecular O—H···S, O—H···N, C—H···S, C—H···O and C—H···N hydrogen bonding interactions (Table 1, Fig. 2).

Related literature top

For structures containing the hexakis(isothiocyanato)nickel(II) tetraanion see: Vicente et al. (1996); Kruger & McKee (1996); Hoffman & Wood (1982).

Experimental top

The title salt was synthesized from the reaction of 5,8-diazoniadispiro[4.2.4.2]tetradecane dibromide (0.034 g, 0.1 mmol) in methanol (5 ml) and a mixture of NiCl₂ (0.013 g, 0.1 mmol) and KNCS(0.074 g, 0.4 mmol) in DMF (10 ml). The resulting mixture was set aside for the formation of green crystals (yield 40%) after several days on slow evaporation of the solvent.

Structure description top

For structures containing the hexakis(isothiocyanato)nickel(II) tetraanion see: Vicente et al. (1996); Kruger & McKee (1996); Hoffman & Wood (1982).

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1994); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXL97.

Figures top

	Fig. 1. Perspective view of the title compound with atom-numbering scheme. Displacement ellipsoids are shown at the 30% probability level. Unlabelled atoms and those with the suffix A are related to labelled atoms by the symmetry operation (2 - x, 1 - y, -z).
	Fig. 2. Packing diagram of the title compound. Dashed lines indicate hydrogen bonding interactions.

Bis(5,8-diazoniadispiro[4.2.4.2]tetradecane) hexakis(thiocyanato-κN)nickel(II) dihydrate top

Crystal data top

(C₁₂H₂₄N₂)₂[Ni(NCS)₆]·2H₂O	F(000) = 884
M_r = 835.89	D_x = 1.407 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5316 reflections
a = 9.959 (6) Å	θ = 2.6–27.3°
b = 13.537 (8) Å	µ = 0.85 mm⁻¹
c = 14.718 (9) Å	T = 273 K
β = 96.186 (10)°	Block, green
V = 1973 (2) Å³	0.30 × 0.15 × 0.15 mm
Z = 2

Data collection top

Siemen SMART CCD diffractometer	3660 independent reflections
Radiation source: fine-focus sealed tube	3220 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.024
ω scan	θ_max = 25.5°, θ_min = 2.1°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→12
T_min = 0.857, T_max = 0.884	k = −16→16
10750 measured reflections	l = −9→17

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.038	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.105	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ²(F_o²) + (0.0548P)² + 0.9458P] where P = (F_o² + 2F_c²)/3
3660 reflections	(Δ/σ)_max < 0.001
231 parameters	Δρ_max = 0.57 e Å⁻³
0 restraints	Δρ_min = −0.40 e Å⁻³

Crystal data top

(C₁₂H₂₄N₂)₂[Ni(NCS)₆]·2H₂O	V = 1973 (2) Å³
M_r = 835.89	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 9.959 (6) Å	µ = 0.85 mm⁻¹
b = 13.537 (8) Å	T = 273 K
c = 14.718 (9) Å	0.30 × 0.15 × 0.15 mm
β = 96.186 (10)°

Data collection top

Siemen SMART CCD diffractometer	3660 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3220 reflections with I > 2σ(I)
T_min = 0.857, T_max = 0.884	R_int = 0.024
10750 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.038	0 restraints
wR(F²) = 0.105	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	Δρ_max = 0.57 e Å⁻³
3660 reflections	Δρ_min = −0.40 e Å⁻³
231 parameters

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Ni1	1.0000	0.5000	0.0000	0.03897 (14)
S1	1.38818 (7)	0.68186 (6)	0.13836 (5)	0.0622 (2)
S2	0.81710 (8)	0.83015 (5)	−0.00780 (6)	0.0666 (2)
S3	0.88411 (6)	0.38952 (5)	0.29815 (4)	0.04961 (18)
O1	0.6492 (3)	0.5411 (2)	0.1087 (3)	0.1166 (12)
N1	1.1787 (2)	0.56492 (16)	0.05640 (15)	0.0542 (5)
N2	0.9026 (2)	0.63532 (16)	0.01364 (15)	0.0535 (5)
N3	0.9581 (2)	0.45753 (16)	0.13052 (14)	0.0502 (5)
N4	0.62283 (18)	0.20076 (14)	0.15891 (13)	0.0422 (4)
N5	0.42206 (17)	0.34300 (13)	0.21603 (12)	0.0364 (4)
C1	1.2661 (2)	0.61201 (17)	0.09023 (16)	0.0439 (5)
C2	0.8688 (2)	0.71628 (17)	0.00460 (14)	0.0394 (5)
C3	0.9277 (2)	0.42916 (16)	0.19955 (16)	0.0387 (5)
C4	0.7825 (3)	0.1334 (3)	0.0665 (2)	0.0785 (10)
H4A	0.8509	0.0824	0.0663	0.094*
H4B	0.8082	0.1886	0.0301	0.094*
C5	0.6463 (3)	0.0939 (2)	0.0289 (2)	0.0677 (8)
H5A	0.6489	0.0224	0.0242	0.081*
H5B	0.6194	0.1211	−0.0313	0.081*
C6	0.5482 (3)	0.12534 (19)	0.0955 (2)	0.0591 (7)
H6A	0.5214	0.0690	0.1300	0.071*
H6B	0.4680	0.1546	0.0630	0.071*
C7	0.7685 (3)	0.1662 (2)	0.1626 (2)	0.0613 (7)
H7A	0.8305	0.2197	0.1807	0.074*
H7B	0.7857	0.1119	0.2053	0.074*
C8	0.5808 (2)	0.20186 (18)	0.25351 (16)	0.0478 (6)
H8A	0.6426	0.2430	0.2923	0.057*
H8B	0.5859	0.1354	0.2782	0.057*
C9	0.4389 (2)	0.24057 (18)	0.25463 (17)	0.0481 (6)
H9A	0.3765	0.1965	0.2194	0.058*
H9B	0.4161	0.2408	0.3171	0.058*
C10	0.6074 (2)	0.30442 (17)	0.12066 (15)	0.0425 (5)
H10A	0.6695	0.3481	0.1565	0.051*
H10B	0.6309	0.3047	0.0584	0.051*
C11	0.4657 (2)	0.34236 (16)	0.12166 (15)	0.0397 (5)
H11A	0.4603	0.4090	0.0972	0.048*
H11B	0.4044	0.3012	0.0824	0.048*
C12	0.4972 (2)	0.4200 (2)	0.27791 (17)	0.0500 (6)
H12A	0.5775	0.3916	0.3110	0.060*
H12B	0.5235	0.4757	0.2424	0.060*
C13	0.4000 (3)	0.4514 (3)	0.3420 (2)	0.0799 (10)
H13A	0.4099	0.4107	0.3966	0.096*
H13B	0.4155	0.5198	0.3598	0.096*
C14	0.2636 (3)	0.4392 (3)	0.2928 (2)	0.0667 (8)
H14A	0.2273	0.5032	0.2732	0.080*
H14B	0.2037	0.4097	0.3329	0.080*
C15	0.2732 (2)	0.37487 (19)	0.21222 (18)	0.0503 (6)
H15A	0.2462	0.4107	0.1562	0.060*
H15B	0.2152	0.3176	0.2147	0.060*
H1B	0.601 (8)	0.604 (6)	0.099 (5)	0.20 (3)*
H1C	0.720 (7)	0.539 (5)	0.061 (4)	0.20 (3)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Ni1	0.0368 (2)	0.0394 (2)	0.0404 (2)	0.00054 (15)	0.00290 (17)	0.00225 (16)
S1	0.0511 (4)	0.0662 (4)	0.0686 (5)	−0.0110 (3)	0.0028 (3)	−0.0142 (3)
S2	0.0639 (4)	0.0423 (4)	0.0884 (6)	0.0048 (3)	−0.0152 (4)	−0.0038 (3)
S3	0.0476 (3)	0.0591 (4)	0.0417 (3)	−0.0066 (3)	0.0031 (3)	0.0020 (3)
O1	0.0871 (19)	0.0908 (19)	0.183 (3)	0.0212 (16)	0.065 (2)	0.043 (2)
N1	0.0489 (12)	0.0552 (12)	0.0569 (13)	−0.0076 (10)	−0.0013 (10)	0.0038 (10)
N2	0.0581 (13)	0.0509 (12)	0.0510 (12)	0.0082 (10)	0.0033 (10)	0.0004 (10)
N3	0.0477 (11)	0.0547 (12)	0.0483 (12)	0.0014 (9)	0.0059 (9)	0.0048 (10)
N4	0.0379 (10)	0.0412 (10)	0.0461 (11)	0.0066 (8)	−0.0014 (8)	−0.0067 (8)
N5	0.0308 (9)	0.0411 (9)	0.0368 (9)	0.0007 (7)	0.0021 (7)	−0.0006 (7)
C1	0.0434 (13)	0.0446 (12)	0.0445 (13)	0.0024 (10)	0.0080 (10)	0.0055 (10)
C2	0.0364 (11)	0.0467 (13)	0.0342 (11)	−0.0010 (9)	0.0002 (9)	−0.0031 (9)
C3	0.0318 (10)	0.0378 (11)	0.0456 (13)	0.0006 (8)	−0.0003 (9)	−0.0036 (10)
C4	0.0634 (18)	0.100 (2)	0.074 (2)	0.0218 (17)	0.0169 (16)	−0.0242 (19)
C5	0.089 (2)	0.0620 (17)	0.0509 (16)	0.0094 (15)	0.0024 (15)	−0.0116 (13)
C6	0.0533 (15)	0.0458 (13)	0.0744 (18)	0.0057 (11)	−0.0102 (13)	−0.0163 (12)
C7	0.0425 (14)	0.0744 (18)	0.0649 (17)	0.0172 (12)	−0.0035 (12)	−0.0142 (14)
C8	0.0520 (14)	0.0454 (13)	0.0451 (13)	0.0080 (10)	0.0016 (11)	0.0114 (10)
C9	0.0470 (13)	0.0511 (13)	0.0471 (13)	−0.0005 (10)	0.0092 (10)	0.0148 (11)
C10	0.0436 (12)	0.0501 (13)	0.0350 (11)	−0.0039 (10)	0.0089 (9)	−0.0003 (9)
C11	0.0445 (12)	0.0391 (11)	0.0349 (11)	0.0008 (9)	0.0011 (9)	0.0046 (9)
C12	0.0400 (12)	0.0589 (14)	0.0504 (14)	−0.0019 (11)	0.0016 (10)	−0.0172 (12)
C13	0.0538 (16)	0.114 (3)	0.071 (2)	0.0186 (17)	0.0001 (15)	−0.0402 (19)
C14	0.0437 (14)	0.090 (2)	0.0682 (18)	0.0034 (14)	0.0135 (13)	−0.0182 (16)
C15	0.0319 (11)	0.0584 (14)	0.0593 (15)	0.0062 (10)	−0.0004 (10)	−0.0016 (12)

Geometric parameters (Å, º) top

Ni1—N1	2.076 (2)	C5—H5A	0.9700
Ni1—N1ⁱ	2.076 (2)	C5—H5B	0.9700
Ni1—N3	2.090 (2)	C6—H6A	0.9700
Ni1—N3ⁱ	2.090 (2)	C6—H6B	0.9700
Ni1—N2	2.093 (2)	C7—H7A	0.9700
Ni1—N2ⁱ	2.093 (2)	C7—H7B	0.9700
S1—C1	1.640 (3)	C8—C9	1.508 (3)
S2—C2	1.629 (3)	C8—H8A	0.9700
S3—C3	1.649 (3)	C8—H8B	0.9700
O1—H1B	0.99 (8)	C9—H9A	0.9700
O1—H1C	1.05 (7)	C9—H9B	0.9700
N1—C1	1.148 (3)	C10—C11	1.503 (3)
N2—C2	1.150 (3)	C10—H10A	0.9700
N3—C3	1.156 (3)	C10—H10B	0.9700
N4—C8	1.497 (3)	C11—H11A	0.9700
N4—C10	1.514 (3)	C11—H11B	0.9700
N4—C7	1.520 (3)	C12—C13	1.485 (4)
N4—C6	1.522 (3)	C12—H12A	0.9700
N5—C11	1.499 (3)	C12—H12B	0.9700
N5—C9	1.501 (3)	C13—C14	1.478 (4)
N5—C12	1.526 (3)	C13—H13A	0.9700
N5—C15	1.539 (3)	C13—H13B	0.9700
C4—C7	1.503 (4)	C14—C15	1.483 (4)
C4—C5	1.507 (5)	C14—H14A	0.9700
C4—H4A	0.9700	C14—H14B	0.9700
C4—H4B	0.9700	C15—H15A	0.9700
C5—C6	1.517 (4)	C15—H15B	0.9700

N1—Ni1—N1ⁱ	180.0	C4—C7—H7A	111.0
N1—Ni1—N3	89.79 (9)	N4—C7—H7A	111.0
N1ⁱ—Ni1—N3	90.21 (9)	C4—C7—H7B	111.0
N1—Ni1—N3ⁱ	90.21 (9)	N4—C7—H7B	111.0
N1ⁱ—Ni1—N3ⁱ	89.79 (9)	H7A—C7—H7B	109.0
N3—Ni1—N3ⁱ	180.00 (11)	N4—C8—C9	111.71 (19)
N1—Ni1—N2	88.70 (10)	N4—C8—H8A	109.3
N1ⁱ—Ni1—N2	91.30 (10)	C9—C8—H8A	109.3
N3—Ni1—N2	90.68 (9)	N4—C8—H8B	109.3
N3ⁱ—Ni1—N2	89.32 (9)	C9—C8—H8B	109.3
N1—Ni1—N2ⁱ	91.30 (10)	H8A—C8—H8B	107.9
N1ⁱ—Ni1—N2ⁱ	88.70 (10)	N5—C9—C8	112.55 (19)
N3—Ni1—N2ⁱ	89.32 (9)	N5—C9—H9A	109.1
N3ⁱ—Ni1—N2ⁱ	90.68 (9)	C8—C9—H9A	109.1
N2—Ni1—N2ⁱ	180.0	N5—C9—H9B	109.1
H1B—O1—H1C	107 (5)	C8—C9—H9B	109.1
C1—N1—Ni1	170.2 (2)	H9A—C9—H9B	107.8
C2—N2—Ni1	162.9 (2)	C11—C10—N4	111.77 (18)
C3—N3—Ni1	174.8 (2)	C11—C10—H10A	109.3
C8—N4—C10	108.03 (17)	N4—C10—H10A	109.3
C8—N4—C7	109.36 (19)	C11—C10—H10B	109.3
C10—N4—C7	110.9 (2)	N4—C10—H10B	109.3
C8—N4—C6	114.2 (2)	H10A—C10—H10B	107.9
C10—N4—C6	111.73 (19)	N5—C11—C10	112.15 (17)
C7—N4—C6	102.51 (18)	N5—C11—H11A	109.2
C11—N5—C9	108.28 (17)	C10—C11—H11A	109.2
C11—N5—C12	112.61 (17)	N5—C11—H11B	109.2
C9—N5—C12	112.18 (19)	C10—C11—H11B	109.2
C11—N5—C15	110.00 (17)	H11A—C11—H11B	107.9
C9—N5—C15	109.93 (18)	C13—C12—N5	105.3 (2)
C12—N5—C15	103.79 (17)	C13—C12—H12A	110.7
N1—C1—S1	178.5 (2)	N5—C12—H12A	110.7
N2—C2—S2	178.5 (2)	C13—C12—H12B	110.7
N3—C3—S3	179.6 (2)	N5—C12—H12B	110.7
C7—C4—C5	106.2 (3)	H12A—C12—H12B	108.8
C7—C4—H4A	110.5	C14—C13—C12	106.5 (2)
C5—C4—H4A	110.5	C14—C13—H13A	110.4
C7—C4—H4B	110.5	C12—C13—H13A	110.4
C5—C4—H4B	110.5	C14—C13—H13B	110.4
H4A—C4—H4B	108.7	C12—C13—H13B	110.4
C4—C5—C6	106.2 (2)	H13A—C13—H13B	108.6
C4—C5—H5A	110.5	C13—C14—C15	108.8 (2)
C6—C5—H5A	110.5	C13—C14—H14A	109.9
C4—C5—H5B	110.5	C15—C14—H14A	109.9
C6—C5—H5B	110.5	C13—C14—H14B	109.9
H5A—C5—H5B	108.7	C15—C14—H14B	109.9
C5—C6—N4	106.2 (2)	H14A—C14—H14B	108.3
C5—C6—H6A	110.5	C14—C15—N5	106.28 (19)
N4—C6—H6A	110.5	C14—C15—H15A	110.5
C5—C6—H6B	110.5	N5—C15—H15A	110.5
N4—C6—H6B	110.5	C14—C15—H15B	110.5
H6A—C6—H6B	108.7	N5—C15—H15B	110.5
C4—C7—N4	104.0 (2)	H15A—C15—H15B	108.7

N1—Ni1—N2—C2	68.3 (7)	C15—N5—C9—C8	175.6 (2)
N1ⁱ—Ni1—N2—C2	−111.7 (7)	N4—C8—C9—N5	−58.1 (3)
N3—Ni1—N2—C2	158.1 (7)	C8—N4—C10—C11	−56.7 (2)
N3ⁱ—Ni1—N2—C2	−21.9 (7)	C7—N4—C10—C11	−176.57 (19)
C7—C4—C5—C6	12.4 (4)	C6—N4—C10—C11	69.7 (2)
C4—C5—C6—N4	11.9 (3)	C9—N5—C11—C10	−55.6 (2)
C8—N4—C6—C5	−149.4 (2)	C12—N5—C11—C10	69.0 (2)
C10—N4—C6—C5	87.6 (2)	C15—N5—C11—C10	−175.73 (18)
C7—N4—C6—C5	−31.2 (3)	N4—C10—C11—N5	58.4 (2)
C5—C4—C7—N4	−32.0 (3)	C11—N5—C12—C13	149.0 (2)
C8—N4—C7—C4	160.3 (2)	C9—N5—C12—C13	−88.6 (3)
C10—N4—C7—C4	−80.7 (3)	C15—N5—C12—C13	30.0 (3)
C6—N4—C7—C4	38.7 (3)	N5—C12—C13—C14	−29.0 (4)
C10—N4—C8—C9	56.3 (2)	C12—C13—C14—C15	16.5 (4)
C7—N4—C8—C9	177.1 (2)	C13—C14—C15—N5	2.7 (4)
C6—N4—C8—C9	−68.7 (3)	C11—N5—C15—C14	−140.7 (2)
C11—N5—C9—C8	55.4 (2)	C9—N5—C15—C14	100.1 (2)
C12—N5—C9—C8	−69.4 (3)	C12—N5—C15—C14	−20.0 (3)

Symmetry code: (i) −x+2, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C10—H10A···S3	0.97	2.88	3.767 (3)	153
C11—H11A···O1	0.97	2.59	3.269 (4)	127
C12—H12B···O1	0.97	2.60	3.463 (5)	149
O1—H1C···N2	1.05 (7)	2.40 (7)	3.273 (4)	139 (5)
C6—H6A···S3ⁱⁱ	0.97	2.77	3.587 (3)	142
C6—H6B···S2ⁱⁱⁱ	0.97	2.88	3.775 (4)	155
C15—H15A···N1^iv	0.97	2.60	3.507 (3)	156
O1—H1B···S1^iv	0.99 (8)	2.49 (8)	3.290 (3)	139 (6)
O1—H1C···N1ⁱ	1.05 (7)	2.52 (7)	3.435 (5)	145 (5)

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

Experimental details

Crystal data
Chemical formula	(C₁₂H₂₄N₂)₂[Ni(NCS)₆]·2H₂O
M_r	835.89
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	273
a, b, c (Å)	9.959 (6), 13.537 (8), 14.718 (9)
β (°)	96.186 (10)
V (Å³)	1973 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.85
Crystal size (mm)	0.30 × 0.15 × 0.15

Data collection
Diffractometer	Siemen SMART CCD
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.857, 0.884
No. of measured, independent and observed [I > 2σ(I)] reflections	10750, 3660, 3220
R_int	0.024
(sin θ/λ)_max (Å⁻¹)	0.606

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.038, 0.105, 1.06
No. of reflections	3660
No. of parameters	231
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.57, −0.40

Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1994), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1994), SHELXL97.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C10—H10A···S3	0.97	2.88	3.767 (3)	153.4
C11—H11A···O1	0.97	2.59	3.269 (4)	127.4
C12—H12B···O1	0.97	2.60	3.463 (5)	148.6
O1—H1C···N2	1.05 (7)	2.40 (7)	3.273 (4)	139 (5)
C6—H6A···S3ⁱ	0.97	2.77	3.587 (3)	142.0
C6—H6B···S2ⁱⁱ	0.97	2.88	3.775 (4)	154.7
C15—H15A···N1ⁱⁱⁱ	0.97	2.60	3.507 (3)	156.0
O1—H1B···S1ⁱⁱⁱ	0.99 (8)	2.49 (8)	3.290 (3)	139 (6)
O1—H1C···N1^iv	1.05 (7)	2.52 (7)	3.435 (5)	145 (5)

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

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