Synthesis, crystal structure and properties of bis­(iso­seleno­cyanato-κN)tetra­kis­(pyridine-κN)nickel(II)

In the crystal structure of the title compound, discrete centrosymmetric complexes are observed, in which the Ni cations are octa­hedrally coordinated by two terminal N-bonded seleno­cyanate anions and four pyridine coligands.

Key indicators

Structure: I

• Single-crystal X-ray study
• T = 170 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.030
• wR factor = 0.075
• Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full value Low .      0.971 Why?
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         62 Report

Alert level G
PLAT012_ALERT_1_G N.O.K.   _shelx_res_checksum Found in CIF ......     Please Check
PLAT230_ALERT_2_G Hirshfeld Test Diff for    Se1      --C1       .        8.2 s.u.
PLAT480_ALERT_4_G Long H...A H-Bond Reported H11      ..SE1      .       3.09 Ang.
PLAT480_ALERT_4_G Long H...A H-Bond Reported H11      ..N1       .       2.67 Ang.
PLAT480_ALERT_4_G Long H...A H-Bond Reported H12      ..SE1      .       3.11 Ang.
PLAT480_ALERT_4_G Long H...A H-Bond Reported H22      ..SE1      .       3.13 Ang.
PLAT480_ALERT_4_G Long H...A H-Bond Reported H25      ..SE1      .       3.00 Ang.
PLAT794_ALERT_5_G Tentative Bond Valency for Ni1       (II)      .       1.90 Info
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         26 Note
PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          1 Note
PLAT941_ALERT_3_G Average HKL Measurement Multiplicity ...........        2.9 Low
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          1 Info

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

   1 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
   4 ALERT type 3 Indicator that the structure quality may be low
   6 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: SHELXT2014/5 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2016/6 (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg & Putz, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis(isoselenocyanato-κN)tetrakis(pyridine-κN)nickel(II)

Crystal data

[Ni(NCSe)2(C5H5N)4]	F(000) = 1160
Mr = 585.07	Dx = 1.654 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 12.4422 (10) Å	Cell parameters from 7129 reflections
b = 13.2302 (9) Å	θ = 2.3–27.0°
c = 15.0723 (12) Å	µ = 3.95 mm^−1
β = 108.755 (9)°	T = 170 K
V = 2349.4 (3) Å^3	Block, purple
Z = 4	0.50 × 0.40 × 0.30 mm

Data collection

Stoe IPDS-2 diffractometer	1971 reflections with I > 2σ(I)
ω scans	Rint = 0.034
Absorption correction: numerical (X-Shape and X-Red 32; Stoe, 2008)	θmax = 27.0°, θmin = 2.3°
Tmin = 0.486, Tmax = 0.563	h = −15→15
7129 measured reflections	k = −13→16
2485 independent reflections	l = −19→19

Refinement

Refinement on F^2	Primary atom site location: dual
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.030	H-atom parameters constrained
wR(F^2) = 0.075	w = 1/[σ^2(Fo^2) + (0.0461P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max < 0.001
2485 reflections	Δρmax = 0.89 e Å^−3
142 parameters	Δρmin = −0.64 e Å^−3
0 restraints

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	0.750000	0.750000	0.500000	0.01661 (12)
N11	0.63560 (19)	0.62770 (17)	0.43798 (16)	0.0204 (5)
C11	0.6697 (3)	0.5310 (2)	0.4492 (2)	0.0277 (6)
H11	0.747512	0.517340	0.481265	0.033*
C12	0.5971 (3)	0.4497 (3)	0.4165 (2)	0.0365 (7)
H12	0.624361	0.382260	0.427221	0.044*
C13	0.4841 (3)	0.4692 (3)	0.3678 (2)	0.0397 (8)
H13	0.432159	0.415397	0.344311	0.048*
C14	0.4487 (3)	0.5685 (3)	0.3543 (3)	0.0391 (8)
H14	0.371805	0.584215	0.320745	0.047*
C15	0.5265 (3)	0.6448 (2)	0.3902 (2)	0.0291 (6)
H15	0.501079	0.712884	0.380325	0.035*
N21	0.78775 (18)	0.68763 (17)	0.63947 (15)	0.0193 (5)
C21	0.7547 (2)	0.7336 (2)	0.7063 (2)	0.0258 (6)
H21	0.716401	0.796653	0.692048	0.031*
C22	0.7742 (3)	0.6931 (3)	0.7948 (2)	0.0312 (7)
H22	0.750093	0.728412	0.839944	0.037*
C23	0.8288 (3)	0.6010 (3)	0.8172 (2)	0.0319 (7)
H23	0.842008	0.571618	0.877261	0.038*
C24	0.8638 (3)	0.5528 (2)	0.7495 (2)	0.0299 (6)
H24	0.901305	0.489356	0.762043	0.036*
C25	0.8428 (2)	0.5993 (2)	0.6628 (2)	0.0244 (6)
H25	0.868951	0.566730	0.617400	0.029*
Se1	0.41596 (3)	0.85023 (2)	0.58223 (2)	0.02991 (11)
C1	0.5366 (2)	0.83774 (19)	0.54277 (18)	0.0196 (5)
N1	0.6154 (2)	0.82749 (18)	0.51901 (16)	0.0228 (5)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0135 (2)	0.0166 (2)	0.0203 (2)	0.00038 (17)	0.0062 (2)	−0.00075 (18)
N11	0.0182 (12)	0.0201 (12)	0.0227 (11)	−0.0014 (9)	0.0061 (10)	−0.0024 (9)
C11	0.0268 (16)	0.0216 (15)	0.0342 (16)	0.0006 (12)	0.0090 (14)	−0.0016 (12)
C12	0.044 (2)	0.0225 (15)	0.0430 (18)	−0.0059 (14)	0.0145 (17)	−0.0052 (14)
C13	0.041 (2)	0.0353 (19)	0.0436 (19)	−0.0199 (15)	0.0143 (17)	−0.0140 (15)
C14	0.0221 (17)	0.041 (2)	0.046 (2)	−0.0095 (13)	0.0004 (16)	−0.0070 (16)
C15	0.0228 (16)	0.0275 (15)	0.0333 (16)	−0.0016 (12)	0.0038 (14)	−0.0019 (12)
N21	0.0173 (12)	0.0204 (11)	0.0201 (11)	−0.0011 (9)	0.0061 (10)	−0.0006 (9)
C21	0.0231 (15)	0.0300 (15)	0.0244 (14)	−0.0004 (11)	0.0078 (13)	−0.0056 (12)
C22	0.0315 (17)	0.0428 (18)	0.0207 (13)	−0.0025 (14)	0.0103 (14)	−0.0067 (13)
C23	0.0279 (17)	0.047 (2)	0.0198 (14)	−0.0048 (14)	0.0059 (14)	0.0037 (13)
C24	0.0295 (16)	0.0296 (16)	0.0301 (14)	0.0048 (13)	0.0088 (14)	0.0073 (13)
C25	0.0242 (16)	0.0243 (15)	0.0249 (14)	0.0029 (11)	0.0079 (13)	−0.0008 (11)
Se1	0.02946 (18)	0.02786 (17)	0.04138 (19)	0.00354 (12)	0.02390 (15)	0.00093 (13)
C1	0.0225 (14)	0.0150 (12)	0.0186 (13)	0.0024 (10)	0.0028 (12)	−0.0001 (10)
N1	0.0186 (12)	0.0235 (12)	0.0270 (12)	0.0028 (9)	0.0084 (11)	0.0007 (9)

Geometric parameters (Å, º)

Ni1—N1^i	2.061 (2)	C14—H14	0.9500
Ni1—N1	2.061 (2)	C15—H15	0.9500
Ni1—N11	2.159 (2)	N21—C25	1.342 (4)
Ni1—N11^i	2.159 (2)	N21—C21	1.350 (3)
Ni1—N21	2.165 (2)	C21—C22	1.384 (4)
Ni1—N21^i	2.165 (2)	C21—H21	0.9500
N11—C15	1.336 (4)	C22—C23	1.383 (5)
N11—C11	1.342 (4)	C22—H22	0.9500
C11—C12	1.388 (4)	C23—C24	1.387 (4)
C11—H11	0.9500	C23—H23	0.9500
C12—C13	1.385 (5)	C24—C25	1.391 (4)
C12—H12	0.9500	C24—H24	0.9500
C13—C14	1.380 (5)	C25—H25	0.9500
C13—H13	0.9500	Se1—C1	1.792 (3)
C14—C15	1.384 (4)	C1—N1	1.154 (3)
N1^i—Ni1—N1	180.0	C13—C14—C15	119.1 (3)
N1^i—Ni1—N11	91.10 (9)	C13—C14—H14	120.4
N1—Ni1—N11	88.90 (9)	C15—C14—H14	120.4
N1^i—Ni1—N11^i	88.90 (9)	N11—C15—C14	123.3 (3)
N1—Ni1—N11^i	91.10 (9)	N11—C15—H15	118.3
N11—Ni1—N11^i	180.00 (8)	C14—C15—H15	118.3
N1^i—Ni1—N21	90.75 (9)	C25—N21—C21	116.7 (2)
N1—Ni1—N21	89.25 (9)	C25—N21—Ni1	121.25 (17)
N11—Ni1—N21	92.40 (8)	C21—N21—Ni1	122.01 (19)
N11^i—Ni1—N21	87.60 (8)	N21—C21—C22	122.9 (3)
N1^i—Ni1—N21^i	89.25 (9)	N21—C21—H21	118.5
N1—Ni1—N21^i	90.75 (9)	C22—C21—H21	118.5
N11—Ni1—N21^i	87.61 (8)	C23—C22—C21	119.8 (3)
N11^i—Ni1—N21^i	92.40 (8)	C23—C22—H22	120.1
N21—Ni1—N21^i	180.0	C21—C22—H22	120.1
C15—N11—C11	117.1 (3)	C22—C23—C24	118.1 (3)
C15—N11—Ni1	121.4 (2)	C22—C23—H23	120.9
C11—N11—Ni1	121.5 (2)	C24—C23—H23	120.9
N11—C11—C12	123.4 (3)	C23—C24—C25	118.7 (3)
N11—C11—H11	118.3	C23—C24—H24	120.7
C12—C11—H11	118.3	C25—C24—H24	120.7
C13—C12—C11	118.5 (3)	N21—C25—C24	123.8 (3)
C13—C12—H12	120.7	N21—C25—H25	118.1
C11—C12—H12	120.7	C24—C25—H25	118.1
C14—C13—C12	118.5 (3)	N1—C1—Se1	178.1 (2)
C14—C13—H13	120.8	C1—N1—Ni1	155.6 (2)
C12—C13—H13	120.8

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C11—H11···Se1^ii	0.95	3.09	3.895 (3)	144
C11—H11···N1^i	0.95	2.67	3.173 (4)	114
C12—H12···Se1^iii	0.95	3.11	3.972 (3)	151
C15—H15···N1	0.95	2.60	3.074 (4)	111
C21—H21···N1	0.95	2.54	3.061 (4)	115
C22—H22···Se1^iv	0.95	3.13	4.022 (3)	157
C25—H25···Se1^ii	0.95	3.00	3.725 (3)	134
C25—H25···N1^i	0.95	2.55	3.103 (4)	118

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