Crystal structure of di­aqua­bis­(2-chloro­pyridine-κN)bis­(thio­cyanato-κN)nickel(II)

The crystal structure of the title compound consists of discrete octa­hedral complexes that are linked by inter­molecular O—H...S, C—H...Cl, C—H...S and C—H...Cl hydrogen bonding.

Key indicators

• Single-crystal X-ray study
• T = 200 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.049
• wR factor = 0.123
• Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT112_ALERT_2_C ADDSYM Detects New (Pseudo) Symm. Elem.        B         83 %Fit
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00775 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H21    ..  S1      ..       2.99 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H23    ..  S1      ..       2.99 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H24    ..  CL1     ..       2.96 Ang.
PLAT906_ALERT_3_C Large K value in the Analysis of Variance ......      9.443 Check
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.596         16 Report
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density           0 Note

Alert level G
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          2 Report
PLAT128_ALERT_4_G Alternate Setting for Input Space Group     C2/c       I2/a Note
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          2 Note
PLAT909_ALERT_3_G Percentage of Observed Data at Theta(Max) Still          73 %
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min)           1 Note
PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          3 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   8 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   6 ALERT level G = General information/check it is not something unexpected

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

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Computing details

Data collection: X-AREA (Stoe, 2008); cell refinement: X-AREA (Stoe, 2008); data reduction: X-AREA (Stoe, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015); molecular graphics: XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Diaquabis(2-chloropyridine-κN)bis(thiocyanato-κN)nickel(II)

Crystal data

[Ni(NCS)2(C5H4ClN)2(H2O)2]	F(000) = 888
Mr = 437.99	Dx = 1.626 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 19.5045 (15) Å	Cell parameters from 7195 reflections
b = 7.5486 (5) Å	θ = 2.8–25.1°
c = 14.9387 (11) Å	µ = 1.63 mm^−1
β = 125.560 (7)°	T = 200 K
V = 1789.3 (3) Å^3	Block, blue
Z = 4	0.14 × 0.09 × 0.06 mm

Data collection

STOE IPDS-1 diffractometer	1321 reflections with I > 2σ(I)
Phi scans	Rint = 0.086
Absorption correction: numerical (X-Red and X-Shape; Stoe, 2008)	θmax = 25.1°, θmin = 2.8°
Tmin = 0.796, Tmax = 0.881	h = −23→23
7195 measured reflections	k = −8→8
1568 independent reflections	l = −17→17

Refinement

Refinement on F^2	Hydrogen site location: mixed
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.049	w = 1/[σ^2(Fo^2) + (0.0887P)^2] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.123	(Δ/σ)max < 0.001
S = 1.03	Δρmax = 0.87 e Å^−3
1568 reflections	Δρmin = −0.87 e Å^−3
107 parameters	Extinction correction: SHELXL-2014/7 (Sheldrick 2015), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0046 (11)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

	x	y	z	Uiso*/Ueq
Ni1	0.2500	0.7500	0.5000	0.0294 (3)
N1	0.2189 (2)	0.5551 (4)	0.3900 (2)	0.0374 (7)
C1	0.2063 (2)	0.4433 (4)	0.3291 (3)	0.0307 (7)
S1	0.18836 (7)	0.28294 (11)	0.24339 (8)	0.0404 (3)
N10	0.1155 (2)	0.7772 (4)	0.4334 (3)	0.0360 (7)
C10	0.0670 (2)	0.9202 (4)	0.4075 (3)	0.0367 (8)
C11	−0.0154 (3)	0.9163 (6)	0.3732 (3)	0.0500 (10)
H21	−0.0466	1.0227	0.3568	0.060*
C12	−0.0520 (3)	0.7528 (6)	0.3630 (4)	0.0586 (12)
H22	−0.1088	0.7447	0.3395	0.070*
C13	−0.0039 (3)	0.6027 (6)	0.3879 (4)	0.0520 (10)
H23	−0.0271	0.4888	0.3814	0.062*
C14	0.0780 (3)	0.6201 (5)	0.4222 (3)	0.0425 (8)
H24	0.1104	0.5153	0.4391	0.051*
Cl1	0.11007 (7)	1.12552 (11)	0.41519 (9)	0.0523 (4)
O1	0.26098 (19)	0.5775 (3)	0.6135 (2)	0.0506 (8)
H1O1	0.2506	0.5933	0.6588	0.076*
H2O1	0.2750	0.4730	0.6262	0.076*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0383 (4)	0.0205 (4)	0.0375 (4)	0.0053 (2)	0.0267 (3)	0.0031 (2)
N1	0.0443 (18)	0.0298 (14)	0.0434 (17)	0.0060 (11)	0.0285 (15)	−0.0008 (12)
C1	0.0350 (18)	0.0247 (15)	0.0417 (19)	0.0052 (12)	0.0276 (17)	0.0077 (13)
S1	0.0613 (7)	0.0251 (4)	0.0505 (6)	−0.0030 (3)	0.0415 (5)	−0.0032 (3)
N10	0.0388 (17)	0.0317 (14)	0.0423 (17)	0.0040 (11)	0.0264 (15)	0.0018 (11)
C10	0.036 (2)	0.0375 (17)	0.0383 (19)	0.0087 (14)	0.0225 (17)	0.0037 (14)
C11	0.036 (2)	0.064 (2)	0.043 (2)	0.0151 (18)	0.019 (2)	0.0064 (18)
C12	0.034 (2)	0.087 (4)	0.050 (3)	−0.0007 (19)	0.022 (2)	−0.004 (2)
C13	0.042 (2)	0.057 (2)	0.054 (3)	−0.0120 (19)	0.026 (2)	−0.0078 (19)
C14	0.042 (2)	0.0371 (18)	0.051 (2)	−0.0066 (14)	0.029 (2)	−0.0054 (15)
Cl1	0.0574 (7)	0.0308 (5)	0.0770 (8)	0.0163 (4)	0.0438 (6)	0.0128 (4)
O1	0.079 (2)	0.0367 (13)	0.0661 (18)	0.0270 (13)	0.0597 (18)	0.0243 (12)

Geometric parameters (Å, º)

Ni1—N1^i	2.018 (3)	C10—Cl1	1.734 (4)
Ni1—N1	2.018 (3)	C11—C12	1.389 (6)
Ni1—O1	2.048 (2)	C11—H21	0.9500
Ni1—O1^i	2.048 (2)	C12—C13	1.377 (6)
Ni1—N10	2.208 (3)	C12—H22	0.9500
Ni1—N10^i	2.208 (3)	C13—C14	1.372 (6)
N1—C1	1.158 (4)	C13—H23	0.9500
C1—S1	1.645 (3)	C14—H24	0.9500
N10—C10	1.336 (4)	O1—H1O1	0.8198
N10—C14	1.352 (4)	O1—H2O1	0.8201
C10—C11	1.375 (6)
N1^i—Ni1—N1	180.0	C14—N10—Ni1	112.9 (2)
N1^i—Ni1—O1	87.27 (12)	N10—C10—C11	124.6 (4)
N1—Ni1—O1	92.73 (12)	N10—C10—Cl1	117.9 (3)
N1^i—Ni1—O1^i	92.73 (12)	C11—C10—Cl1	117.4 (3)
N1—Ni1—O1^i	87.27 (12)	C10—C11—C12	118.3 (4)
O1—Ni1—O1^i	180.0	C10—C11—H21	120.8
N1^i—Ni1—N10	90.88 (11)	C12—C11—H21	120.8
N1—Ni1—N10	89.12 (11)	C13—C12—C11	118.4 (4)
O1—Ni1—N10	87.55 (11)	C13—C12—H22	120.8
O1^i—Ni1—N10	92.45 (11)	C11—C12—H22	120.8
N1^i—Ni1—N10^i	89.11 (11)	C14—C13—C12	119.0 (4)
N1—Ni1—N10^i	90.88 (11)	C14—C13—H23	120.5
O1—Ni1—N10^i	92.45 (11)	C12—C13—H23	120.5
O1^i—Ni1—N10^i	87.55 (11)	N10—C14—C13	124.0 (4)
N10—Ni1—N10^i	180.0	N10—C14—H24	118.0
C1—N1—Ni1	175.7 (3)	C13—C14—H24	118.0
N1—C1—S1	179.4 (3)	Ni1—O1—H1O1	129.3
C10—N10—C14	115.6 (3)	Ni1—O1—H2O1	131.5
C10—N10—Ni1	131.4 (2)	H1O1—O1—H2O1	99.1

Symmetry code: (i) −x+1/2, −y+3/2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C11—H21···S1^ii	0.95	2.99	3.904 (4)	162
C13—H23···S1^iii	0.95	2.99	3.796 (4)	143
C14—H24···Cl1^iv	0.95	2.96	3.796 (4)	147
O1—H1O1···S1^v	0.82	2.39	3.175 (2)	160
O1—H2O1···S1^vi	0.82	2.53	3.239 (2)	145
O1—H2O1···Cl1^i	0.82	2.75	3.180 (3)	115

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