Di­chloro­tetrakis(3-hydroxy­pyridine-κN)­nickel(II)

In the title complex, [NiCl₂(C₅H₅NO)₄], the Ni^II atom lies on a special position with twofold rotation symmetry and assumes an elongated octahedral NiN₄Cl₂ configuration defined by two Cl⁻ ions occupying the axial sites [Ni—Cl = 2.4953 (8) Å] and four N atoms of 3-hydroxy­pyridine ligands in the equatorial plane [average Ni—N = 2.119 (2) Å]. A two-dimensional hydrogen-bonding framework is formed by O—H...Cl interactions.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.047
• wR factor = 0.105
• Data-to-parameter ratio = 17.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.05

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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: SHELXL97.

Dichlorotetrakis(3-hydroxypyridine-κN)nickel(II)

Crystal data

[NiCl2(C5H5NO)4]	F(000) = 1048
Mr = 509.99	Dx = 1.524 Mg m^−3
Orthorhombic, Pcca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2a 2ac	Cell parameters from 11124 reflections
a = 15.701 (3) Å	θ = 3.4–27.5°
b = 7.6110 (15) Å	µ = 1.15 mm^−1
c = 18.606 (4) Å	T = 293 K
V = 2223.4 (8) Å^3	Prism, green
Z = 4	0.42 × 0.32 × 0.24 mm

Data collection

Rigaku R-AXIS RAPID diffractometer	2539 independent reflections
Radiation source: fine-focus sealed tube	1944 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.064
Detector resolution: 10 pixels mm^-1	θmax = 27.5°, θmin = 3.2°
ω scans	h = −20→20
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −9→9
Tmin = 0.638, Tmax = 0.762	l = −24→23
19465 measured reflections

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)] = 0.047	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.105	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0482P)^2 + 1.2106P] where P = (Fo^2 + 2Fc^2)/3
2539 reflections	(Δ/σ)max < 0.001
147 parameters	Δρmax = 0.48 e Å^−3
2 restraints	Δρmin = −0.29 e Å^−3

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

	x	y	z	Uiso*/Ueq
Ni1	0.7500	0.0000	0.37573 (2)	0.02804 (14)
Cl1	0.85279 (4)	0.24969 (9)	0.37765 (3)	0.03824 (18)
O1	0.45757 (13)	0.2388 (3)	0.48538 (10)	0.0485 (5)
H11	0.429 (2)	0.258 (5)	0.5231 (12)	0.073*
O2	0.61294 (19)	0.5629 (3)	0.23570 (11)	0.0641 (7)
H12	0.623 (3)	0.619 (5)	0.2742 (14)	0.096*
N1	0.67860 (13)	0.1340 (3)	0.45487 (11)	0.0321 (5)
N2	0.67759 (14)	0.1258 (3)	0.29400 (10)	0.0323 (5)
C1	0.59407 (16)	0.1487 (3)	0.44856 (12)	0.0310 (5)
H1	0.5682	0.1015	0.4079	0.037*
C2	0.54285 (17)	0.2302 (3)	0.49919 (13)	0.0328 (5)
C3	0.58076 (18)	0.2961 (4)	0.56023 (14)	0.0403 (7)
H3	0.5483	0.3484	0.5961	0.048*
C4	0.66840 (19)	0.2826 (4)	0.56691 (15)	0.0464 (7)
H4	0.6954	0.3280	0.6073	0.056*
C5	0.71553 (18)	0.2022 (4)	0.51405 (14)	0.0405 (6)
H5	0.7743	0.1946	0.5192	0.049*
C6	0.66498 (16)	0.3007 (3)	0.29309 (13)	0.0318 (5)
H6	0.6845	0.3667	0.3318	0.038*
C7	0.62442 (19)	0.3871 (4)	0.23750 (14)	0.0396 (6)
C8	0.5957 (2)	0.2883 (4)	0.18033 (15)	0.0537 (9)
H8	0.5689	0.3418	0.1415	0.064*
C9	0.6074 (2)	0.1086 (4)	0.18172 (15)	0.0535 (8)
H9	0.5876	0.0398	0.1439	0.064*
C10	0.6478 (2)	0.0320 (4)	0.23845 (14)	0.0426 (7)
H10	0.6550	−0.0893	0.2386	0.051*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0320 (2)	0.0324 (2)	0.0197 (2)	0.00459 (19)	0.000	0.000
Cl1	0.0418 (3)	0.0417 (4)	0.0313 (3)	−0.0049 (3)	−0.0059 (3)	0.0080 (3)
O1	0.0381 (10)	0.0754 (15)	0.0321 (9)	0.0137 (10)	0.0033 (9)	−0.0028 (10)
O2	0.121 (2)	0.0323 (12)	0.0393 (11)	0.0132 (13)	−0.0272 (13)	−0.0024 (9)
N1	0.0346 (11)	0.0381 (13)	0.0236 (9)	0.0029 (9)	−0.0001 (9)	−0.0028 (9)
N2	0.0394 (12)	0.0341 (12)	0.0235 (9)	0.0044 (9)	−0.0050 (9)	−0.0014 (9)
C1	0.0358 (13)	0.0342 (14)	0.0230 (11)	0.0015 (11)	−0.0017 (10)	−0.0017 (10)
C2	0.0378 (13)	0.0324 (14)	0.0283 (12)	0.0047 (11)	0.0041 (11)	0.0035 (10)
C3	0.0479 (16)	0.0429 (17)	0.0301 (12)	−0.0007 (13)	0.0106 (12)	−0.0105 (11)
C4	0.0513 (17)	0.058 (2)	0.0299 (13)	−0.0088 (14)	−0.0011 (13)	−0.0176 (13)
C5	0.0383 (14)	0.0527 (18)	0.0307 (12)	−0.0021 (13)	−0.0028 (12)	−0.0076 (12)
C6	0.0396 (14)	0.0324 (14)	0.0234 (11)	0.0013 (11)	−0.0037 (11)	−0.0025 (10)
C7	0.0584 (17)	0.0300 (14)	0.0304 (12)	0.0038 (13)	−0.0073 (13)	−0.0005 (11)
C8	0.086 (2)	0.0423 (19)	0.0326 (14)	0.0099 (16)	−0.0255 (16)	−0.0008 (13)
C9	0.084 (2)	0.0422 (18)	0.0347 (14)	0.0047 (16)	−0.0242 (16)	−0.0102 (13)
C10	0.0626 (18)	0.0310 (15)	0.0343 (13)	0.0055 (13)	−0.0119 (14)	−0.0061 (11)

Geometric parameters (Å, º)

Ni1—Cl1	2.4935 (8)	C1—H1	0.9300
Ni1—N1	2.113 (2)	C2—C3	1.377 (4)
Ni1—N2	2.126 (2)	C3—C4	1.385 (4)
O1—C2	1.365 (3)	C3—H3	0.9300
O2—C7	1.351 (4)	C4—C5	1.374 (4)
Ni1—Cl1^i	2.4935 (8)	C4—H4	0.9300
Ni1—N1^i	2.113 (2)	C5—H5	0.9300
Ni1—N2^i	2.126 (2)	C6—C7	1.381 (3)
N1—C1	1.337 (3)	C6—H6	0.9300
N1—C5	1.348 (3)	C7—C8	1.379 (4)
N2—C6	1.346 (3)	C8—C9	1.380 (4)
N2—C10	1.340 (3)	C8—H8	0.9300
O1—H11	0.85 (3)	C9—C10	1.363 (4)
O2—H12	0.85 (3)	C9—H9	0.9300
C1—C2	1.385 (3)	C10—H10	0.9300
Cl1—Ni1—Cl1^i	178.36 (3)	C1—N1—C5	117.8 (2)
N1^i—Ni1—N1	91.67 (11)	C1—N1—Ni1	120.38 (16)
N1^i—Ni1—N2^i	89.85 (8)	C2—O1—H11	112 (3)
N1—Ni1—N2^i	177.84 (9)	C2—C1—H1	118.2
N2^i—Ni1—N2	88.68 (11)	C2—C3—C4	118.4 (2)
N1^i—Ni1—Cl1	90.83 (6)	C2—C3—H3	120.8
N1—Ni1—Cl1	88.02 (6)	C3—C2—C1	118.2 (2)
N2^i—Ni1—Cl1	90.42 (6)	C3—C4—H4	119.9
N2—Ni1—Cl1	90.76 (6)	C4—C3—H3	120.8
N1^i—Ni1—Cl1^i	88.02 (6)	C4—C5—H5	119.2
N1—Ni1—Cl1^i	90.83 (6)	C5—N1—Ni1	121.77 (18)
N1^i—Ni1—N2	177.84 (8)	C5—C4—C3	120.2 (3)
N1—Ni1—N2	89.85 (8)	C5—C4—H4	119.9
N1—C1—C2	123.6 (2)	C6—N2—Ni1	122.20 (16)
N1—C1—H1	118.2	C7—O2—H12	117 (3)
N1—C5—C4	121.6 (3)	C7—C6—H6	118.4
N1—C5—H5	119.2	C7—C8—C9	118.9 (3)
N2^i—Ni1—Cl1^i	90.76 (6)	C7—C8—H8	120.6
N2—Ni1—Cl1^i	90.42 (6)	C8—C7—C6	118.0 (3)
N2—C6—C7	123.2 (2)	C8—C9—H9	120.0
N2—C6—H6	118.4	C9—C8—H8	120.6
N2—C10—C9	122.1 (3)	C9—C10—H10	118.9
N2—C10—H10	118.9	C10—C9—C8	120.0 (3)
O1—C2—C3	124.2 (2)	C10—C9—H9	120.0
O1—C2—C1	117.6 (2)	C10—N2—C6	117.7 (2)
O2—C7—C8	118.5 (2)	C10—N2—Ni1	119.89 (18)
O2—C7—C6	123.5 (2)
Ni1—N1—C1—C2	178.13 (19)	N2—Ni1—N1—C1	43.1 (2)
Ni1—N1—C5—C4	−177.1 (2)	N2—Ni1—N1—C5	−139.1 (2)
Ni1—N2—C6—C7	174.3 (2)	N2^i—Ni1—N2—C6	−128.5 (2)
Ni1—N2—C10—C9	−174.3 (3)	N2^i—Ni1—N2—C10	46.81 (19)
Cl1—Ni1—N1—C1	133.9 (2)	N2—C6—C7—O2	−178.8 (3)
Cl1^i—Ni1—N1—C1	−47.3 (2)	N2—C6—C7—C8	0.0 (4)
Cl1—Ni1—N2—C6	−38.15 (19)	O1—C2—C3—C4	−178.5 (3)
Cl1^i—Ni1—N2—C6	140.71 (19)	O2—C7—C8—C9	179.9 (3)
Cl1—Ni1—N1—C5	−48.3 (2)	C1—C2—C3—C4	2.0 (4)
Cl1^i—Ni1—N1—C5	130.5 (2)	C1—N1—C5—C4	0.7 (4)
Cl1—Ni1—N2—C10	137.2 (2)	C2—C3—C4—C5	−1.1 (5)
Cl1^i—Ni1—N2—C10	−43.9 (2)	C3—C4—C5—N1	−0.3 (5)
N1^i—Ni1—N1—C1	−135.3 (2)	C5—N1—C1—C2	0.3 (4)
N1^i—Ni1—N1—C5	42.47 (18)	C6—N2—C10—C9	1.2 (4)
N1—Ni1—N2—C10	−134.8 (2)	C6—C7—C8—C9	1.1 (5)
N1—Ni1—N2—C6	49.9 (2)	C7—C8—C9—C10	−1.0 (6)
N1—C1—C2—O1	178.8 (2)	C8—C9—C10—N2	−0.2 (5)
N1—C1—C2—C3	−1.7 (4)	C10—N2—C6—C7	−1.1 (4)

Symmetry code: (i) −x+3/2, −y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H11···Cl1^ii	0.85 (3)	2.20 (3)	3.034 (2)	168 (4)
O2—H12···Cl1^iii	0.85 (3)	2.20 (3)	3.050 (2)	177 (4)

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