Diazido­dipyridine­nickel(II)

The title compound, [Ni(N₃)₂(C₅H₅N)₂], has two half-mol­ecules in the asymmetric unit. One complete molecule is generated by twofold symmetry, the other by inversion. In this mononuclear compound, each Ni^II atom is coordinated by four N atoms from two pyridine mol­ecules and two azide anions, thereby forming a slightly distorted square planar configuration.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.040
• wR factor = 0.105
• Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT230_ALERT_2_C Hirshfeld Test Diff for    C5     -   C6      ..       5.38 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Ni2    -   N6      ..       6.60 su
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N4
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N8

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

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 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: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

Diazidodipyridinenickel(II)

Crystal data

[Ni(N3)2(C5H5N)2]	F(000) = 1232
Mr = 300.95	Dx = 1.588 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -c 2yc	Cell parameters from 3601 reflections
a = 12.7646 (16) Å	θ = 1.5–26.5°
b = 14.1998 (16) Å	µ = 1.54 mm^−1
c = 14.1347 (17) Å	T = 293 K
β = 100.766 (3)°	Block, blue
V = 2516.9 (5) Å^3	0.35 × 0.31 × 0.20 mm
Z = 8

Data collection

Bruker SMART CCD area-detector diffractometer	2593 independent reflections
Radiation source: fine-focus sealed tube	2061 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.070
ω scans	θmax = 26.5°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→16
Tmin = 0.589, Tmax = 0.735	k = −17→17
6765 measured reflections	l = −17→10

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)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.105	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0471P)^2 + 0.0859P] where P = (Fo^2 + 2Fc^2)/3
2593 reflections	(Δ/σ)max < 0.001
176 parameters	Δρmax = 0.29 e Å^−3
152 restraints	Δρmin = −0.48 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.5000	0.27065 (3)	0.7500	0.04009 (18)
Ni2	0.2500	0.2500	0.5000	0.04146 (18)
N1	0.5000	0.1258 (2)	0.7500	0.0503 (8)
N2	0.5000	0.4166 (2)	0.7500	0.0491 (8)
N3	0.55407 (19)	0.27085 (15)	0.89221 (17)	0.0482 (6)
N4	0.4931 (2)	0.25992 (14)	0.94727 (19)	0.0431 (6)
N5	0.4382 (2)	0.24990 (19)	1.0016 (2)	0.0733 (9)
N6	0.25379 (17)	0.11101 (15)	0.53003 (17)	0.0449 (5)
N7	0.31177 (19)	0.22258 (16)	0.38266 (19)	0.0538 (6)
N8	0.2542 (2)	0.22687 (15)	0.30438 (19)	0.0465 (6)
N9	0.2010 (3)	0.2280 (2)	0.2300 (2)	0.0800 (9)
C1	0.4236 (3)	0.0770 (2)	0.7815 (2)	0.0659 (9)
H1	0.3701	0.1098	0.8040	0.079*
C2	0.4213 (3)	−0.0198 (2)	0.7817 (3)	0.0872 (12)
H2	0.3666	−0.0517	0.8033	0.105*
C3	0.5000	−0.0684 (4)	0.7500	0.0939 (19)
H3	0.5000	−0.1339	0.7500	0.113*
C4	0.5786 (2)	0.4645 (2)	0.8045 (2)	0.0585 (8)
H4	0.6332	0.4310	0.8429	0.070*
C5	0.5828 (3)	0.5621 (2)	0.8065 (2)	0.0742 (10)
H5	0.6392	0.5939	0.8444	0.089*
C6	0.5000	0.6101 (3)	0.7500	0.0867 (17)
H6	0.5000	0.6756	0.7500	0.104*
C7	0.1713 (2)	0.0679 (2)	0.5585 (2)	0.0530 (7)
H7	0.1148	0.1042	0.5711	0.064*
C8	0.1678 (3)	−0.0289 (2)	0.5699 (2)	0.0644 (9)
H8	0.1093	−0.0572	0.5889	0.077*
C9	0.2522 (3)	−0.0829 (2)	0.5527 (2)	0.0654 (9)
H9	0.2515	−0.1480	0.5597	0.078*
C10	0.3378 (3)	−0.0382 (2)	0.5251 (2)	0.0628 (9)
H10	0.3962	−0.0728	0.5140	0.075*
C11	0.3356 (2)	0.05782 (19)	0.5141 (2)	0.0531 (8)
H11	0.3932	0.0873	0.4949	0.064*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0512 (3)	0.0362 (3)	0.0319 (3)	0.000	0.0053 (2)	0.000
Ni2	0.0548 (3)	0.0354 (3)	0.0372 (3)	0.0018 (2)	0.0167 (3)	−0.0008 (2)
N1	0.067 (2)	0.0421 (18)	0.043 (2)	0.000	0.0137 (17)	0.000
N2	0.059 (2)	0.0453 (18)	0.043 (2)	0.000	0.0098 (17)	0.000
N3	0.0507 (15)	0.0540 (14)	0.0391 (14)	−0.0033 (11)	0.0065 (12)	0.0012 (11)
N4	0.0464 (14)	0.0377 (12)	0.0440 (15)	−0.0003 (9)	0.0055 (13)	0.0022 (10)
N5	0.073 (2)	0.088 (2)	0.065 (2)	−0.0014 (15)	0.0277 (18)	0.0100 (15)
N6	0.0505 (14)	0.0449 (13)	0.0396 (13)	−0.0013 (10)	0.0089 (11)	−0.0010 (11)
N7	0.0545 (16)	0.0620 (15)	0.0476 (17)	0.0076 (12)	0.0162 (13)	−0.0040 (12)
N8	0.0556 (16)	0.0428 (13)	0.0433 (17)	0.0042 (11)	0.0152 (14)	−0.0062 (11)
N9	0.082 (2)	0.106 (2)	0.047 (2)	0.0177 (17)	−0.0008 (17)	−0.0150 (17)
C1	0.085 (2)	0.0548 (19)	0.062 (2)	−0.0102 (17)	0.0236 (18)	−0.0005 (16)
C2	0.124 (3)	0.059 (2)	0.079 (3)	−0.028 (2)	0.023 (3)	0.008 (2)
C3	0.138 (5)	0.053 (3)	0.088 (4)	0.000	0.015 (4)	0.000
C4	0.070 (2)	0.0579 (19)	0.0416 (18)	−0.0076 (15)	−0.0047 (16)	0.0020 (15)
C5	0.098 (3)	0.060 (2)	0.057 (2)	−0.0187 (18)	−0.003 (2)	−0.0029 (17)
C6	0.122 (4)	0.050 (3)	0.093 (4)	0.000	0.033 (4)	0.000
C7	0.0588 (18)	0.0567 (18)	0.0446 (18)	−0.0022 (14)	0.0128 (15)	0.0058 (14)
C8	0.081 (2)	0.0575 (19)	0.057 (2)	−0.0120 (17)	0.0195 (18)	0.0083 (16)
C9	0.095 (3)	0.0448 (17)	0.054 (2)	−0.0028 (17)	0.0094 (19)	0.0061 (15)
C10	0.070 (2)	0.0501 (18)	0.067 (2)	0.0090 (15)	0.0087 (18)	−0.0022 (16)
C11	0.0538 (17)	0.0481 (16)	0.056 (2)	0.0004 (13)	0.0081 (15)	−0.0008 (14)

Geometric parameters (Å, º)

Ni1—N3	2.000 (2)	C2—C3	1.362 (4)
Ni1—N3^i	2.000 (2)	C2—H2	0.9300
Ni1—N1	2.057 (3)	C3—C2^i	1.362 (5)
Ni1—N2	2.073 (3)	C3—H3	0.9300
Ni2—N7^ii	2.003 (2)	C4—C5	1.387 (4)
Ni2—N7	2.003 (2)	C4—H4	0.9300
Ni2—N6^ii	2.017 (2)	C5—C6	1.380 (3)
Ni2—N6	2.017 (2)	C5—H5	0.9300
N1—C1	1.339 (3)	C6—C5^i	1.380 (3)
N1—C1^i	1.339 (3)	C6—H6	0.9300
N2—C4^i	1.332 (3)	C7—C8	1.386 (4)
N2—C4	1.332 (3)	C7—H7	0.9300
N3—N4	1.209 (3)	C8—C9	1.380 (4)
N4—N5	1.141 (4)	C8—H8	0.9300
N6—C11	1.341 (3)	C9—C10	1.381 (4)
N6—C7	1.343 (3)	C9—H9	0.9300
N7—N8	1.210 (3)	C10—C11	1.372 (4)
N8—N9	1.140 (4)	C10—H10	0.9300
C1—C2	1.375 (5)	C11—H11	0.9300
C1—H1	0.9300
N3—Ni1—N3^i	179.84 (13)	C3—C2—H2	120.4
N3—Ni1—N1	90.08 (6)	C1—C2—H2	120.4
N3^i—Ni1—N1	90.08 (6)	C2^i—C3—C2	119.0 (5)
N3—Ni1—N2	89.92 (6)	C2^i—C3—H3	120.5
N3^i—Ni1—N2	89.92 (6)	C2—C3—H3	120.5
N1—Ni1—N2	180.00	N2—C4—C5	123.0 (3)
N7^ii—Ni2—N7	180.0	N2—C4—H4	118.5
N7^ii—Ni2—N6^ii	89.22 (9)	C5—C4—H4	118.5
N7—Ni2—N6^ii	90.78 (9)	C6—C5—C4	117.3 (3)
N7^ii—Ni2—N6	90.78 (9)	C6—C5—H5	121.3
N7—Ni2—N6	89.22 (9)	C4—C5—H5	121.3
N6^ii—Ni2—N6	180.0	C5^i—C6—C5	120.8 (4)
C1—N1—C1^i	117.7 (4)	C5^i—C6—H6	119.6
C1—N1—Ni1	121.15 (19)	C5—C6—H6	119.6
C1^i—N1—Ni1	121.15 (19)	N6—C7—C8	122.0 (3)
C4^i—N2—C4	118.6 (4)	N6—C7—H7	119.0
C4^i—N2—Ni1	120.71 (18)	C8—C7—H7	119.0
C4—N2—Ni1	120.71 (18)	C9—C8—C7	119.2 (3)
N4—N3—Ni1	120.3 (2)	C9—C8—H8	120.4
N5—N4—N3	177.9 (3)	C7—C8—H8	120.4
C11—N6—C7	118.2 (2)	C8—C9—C10	118.7 (3)
C11—N6—Ni2	120.31 (18)	C8—C9—H9	120.7
C7—N6—Ni2	121.28 (19)	C10—C9—H9	120.7
N8—N7—Ni2	118.8 (2)	C11—C10—C9	119.1 (3)
N9—N8—N7	177.8 (3)	C11—C10—H10	120.4
N1—C1—C2	122.3 (3)	C9—C10—H10	120.4
N1—C1—H1	118.8	N6—C11—C10	122.8 (3)
C2—C1—H1	118.8	N6—C11—H11	118.6
C3—C2—C1	119.3 (4)	C10—C11—H11	118.6

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···N9^ii	0.93	2.49	3.182 (5)	131

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