Di-μ-bromo-bis­{aqua­[(5-bromo-1H-imidazol-4-ylmethyl­ene)(2-pyridylmeth­yl)amine-κ³N,N′,N′′]nickel(II)} dibromide

In the title compound, [Ni₂Br₂(C₁₀H₉BrN₄)₂(H₂O)₂]Br₂, the asymmetric unit consists of one half-cation and one Br⁻ anion. The dinuclear cation is located on an inversion centre and each Ni^II ion is chelated by one tridentate (5-bromo-1H-imidazol-4-ylmethyl­ene)(2-pyridylmeth­yl)amine (BIPI) ligand, one water mol­ecule and two bridging Br⁻ ligands. The tridentate BIPI ligand is essentially planar. Hydrogen bonds involving the Br⁻ anions stabilize the crystal structure.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.015 Å
• R factor = 0.043
• wR factor = 0.128
• Data-to-parameter ratio = 17.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         C6
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C5
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...         15

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

   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
   1 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

---

Computing details

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1985); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Di-µ-bromo-bis{aqua[(5-bromo-1H-imidazol-4-ylmethylene)(2-pyridylmethyl)amine- κ³N,N',N'']nickel(II)} dibromide

Crystal data

[Ni2Br2(C10H9BrN4)2(H2O)2]Br2	Z = 1
Mr = 1003.24	F(000) = 480
Triclinic, P1	Dx = 2.207 Mg m^−3
Hall symbol: -P 1	Melting point: 506 K
a = 8.4833 (17) Å	Mo Kα radiation, λ = 0.71073 Å
b = 9.4187 (19) Å	Cell parameters from 25 reflections
c = 10.748 (2) Å	θ = 16.9–26.8°
α = 90.16 (3)°	µ = 9.22 mm^−1
β = 107.77 (3)°	T = 298 K
γ = 111.40 (3)°	Prism, green
V = 755.1 (3) Å^3	0.2 × 0.15 × 0.15 mm

Data collection

Rigaku AFC-7S diffractometer	1603 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.039
Graphite monochromator	θmax = 26.0°, θmin = 2.0°
ω/2θ scans	h = −10→0
Absorption correction: ψ scan (North et al., 1968)	k = −10→11
Tmin = 0.196, Tmax = 0.252	l = −12→13
3189 measured reflections	3 standard reflections every 150 reflections
2977 independent reflections	intensity decay: 0.5%

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)] = 0.043	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.128	H-atom parameters constrained
S = 0.95	w = 1/[σ^2(Fo^2) + (0.0625P)^2] where P = (Fo^2 + 2Fc^2)/3
2977 reflections	(Δ/σ)max < 0.001
172 parameters	Δρmax = 0.71 e Å^−3
0 restraints	Δρmin = −0.85 e Å^−3

Special details

Experimental. The scan width was 1.42 + 0.30tanθ)° with an ω scan speed of 16° per minute (up to 5 scans to achieve I/σ(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1.

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	0.07931 (14)	0.10344 (11)	0.16618 (11)	0.0342 (3)
Br1	0.14088 (12)	0.15998 (9)	−0.05372 (9)	0.0402 (2)
Br2	0.82620 (14)	0.26096 (13)	0.48128 (11)	0.0638 (3)
Br3	0.28619 (13)	0.27035 (10)	0.61345 (10)	0.0490 (3)
N1	−0.0806 (9)	0.2305 (8)	0.1323 (7)	0.0430 (18)
N2	0.2629 (9)	0.3116 (7)	0.2584 (7)	0.0376 (16)
N3	0.3064 (9)	0.0500 (7)	0.2466 (7)	0.0412 (18)
N4	0.5402 (10)	−0.0093 (9)	0.3369 (8)	0.054 (2)
H4A	0.6039	−0.0640	0.3595	0.065*
O1	0.0103 (9)	0.0483 (6)	0.3350 (6)	0.0567 (18)
H1W	0.0762	0.0818	0.4088	0.068*
H2W	−0.0534	−0.0397	0.3525	0.068*
C1	−0.2567 (12)	0.1804 (10)	0.0714 (10)	0.050 (2)
H1	−0.3180	0.0767	0.0384	0.060*
C2	−0.3540 (14)	0.2724 (11)	0.0541 (10)	0.057 (3)
H2	−0.4767	0.2326	0.0091	0.069*
C3	−0.2648 (13)	0.4242 (12)	0.1052 (12)	0.063 (3)
H3	−0.3271	0.4889	0.0968	0.076*
C4	−0.0827 (14)	0.4807 (10)	0.1690 (10)	0.057 (3)
H4	−0.0202	0.5837	0.2038	0.068*
C5	0.0050 (11)	0.3820 (8)	0.1802 (8)	0.038 (2)
C6	0.2041 (13)	0.4392 (10)	0.2533 (12)	0.062 (3)
H6A	0.2684	0.5179	0.2088	0.074*
H6B	0.2298	0.4844	0.3421	0.074*
C7	0.4182 (12)	0.3208 (9)	0.3217 (8)	0.039 (2)
H7	0.5083	0.4133	0.3669	0.047*
C8	0.4498 (11)	0.1802 (9)	0.3204 (8)	0.039 (2)
C9	0.5940 (12)	0.1437 (10)	0.3735 (9)	0.044 (2)
C10	0.3656 (13)	−0.0594 (10)	0.2575 (10)	0.052 (3)
H10	0.2977	−0.1597	0.2164	0.063*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0337 (6)	0.0239 (5)	0.0423 (7)	0.0100 (4)	0.0099 (5)	0.0007 (4)
Br1	0.0400 (5)	0.0273 (4)	0.0482 (6)	0.0074 (4)	0.0141 (4)	0.0019 (4)
Br2	0.0407 (6)	0.0775 (7)	0.0636 (7)	0.0247 (5)	0.0017 (5)	−0.0045 (6)
Br3	0.0479 (6)	0.0316 (5)	0.0591 (6)	0.0095 (4)	0.0135 (5)	0.0039 (4)
N1	0.039 (4)	0.039 (4)	0.051 (5)	0.015 (3)	0.015 (4)	0.004 (3)
N2	0.030 (4)	0.030 (3)	0.046 (4)	0.010 (3)	0.005 (3)	−0.004 (3)
N3	0.033 (4)	0.034 (4)	0.054 (5)	0.012 (3)	0.012 (4)	−0.002 (3)
N4	0.052 (5)	0.047 (4)	0.064 (6)	0.029 (4)	0.009 (4)	0.004 (4)
O1	0.066 (4)	0.039 (3)	0.046 (4)	−0.005 (3)	0.022 (3)	0.000 (3)
C1	0.043 (6)	0.038 (5)	0.066 (7)	0.015 (4)	0.016 (5)	−0.002 (4)
C2	0.045 (6)	0.055 (6)	0.070 (7)	0.024 (5)	0.009 (5)	0.003 (5)
C3	0.043 (6)	0.056 (6)	0.095 (9)	0.029 (5)	0.014 (6)	0.009 (6)
C4	0.073 (7)	0.029 (5)	0.075 (7)	0.029 (5)	0.024 (6)	0.005 (5)
C5	0.038 (5)	0.022 (4)	0.050 (6)	0.009 (4)	0.014 (4)	0.003 (4)
C6	0.050 (6)	0.026 (4)	0.100 (9)	0.015 (4)	0.012 (6)	0.000 (5)
C7	0.040 (5)	0.024 (4)	0.043 (5)	0.005 (4)	0.009 (4)	0.004 (4)
C8	0.033 (4)	0.043 (5)	0.033 (5)	0.014 (4)	0.000 (4)	0.002 (4)
C9	0.043 (5)	0.047 (5)	0.045 (6)	0.020 (4)	0.015 (4)	0.005 (4)
C10	0.057 (6)	0.032 (5)	0.062 (6)	0.016 (4)	0.013 (5)	0.000 (4)

Geometric parameters (Å, º)

Ni1—N2	2.017 (6)	O1—H1W	0.8006
Ni1—N1	2.071 (7)	O1—H2W	0.8662
Ni1—O1	2.082 (6)	C1—C2	1.377 (13)
Ni1—N3	2.099 (7)	C1—H1	0.9300
Ni1—Br1^i	2.5157 (17)	C2—C3	1.367 (13)
Ni1—Br1	2.5884 (16)	C2—H2	0.9300
Br1—Ni1^i	2.5157 (17)	C3—C4	1.376 (13)
Br2—C9	1.858 (9)	C3—H3	0.9300
N1—C1	1.331 (11)	C4—C5	1.372 (11)
N1—C5	1.356 (10)	C4—H4	0.9300
N2—C7	1.255 (10)	C5—C6	1.511 (12)
N2—C6	1.456 (10)	C6—H6A	0.9700
N3—C10	1.292 (10)	C6—H6B	0.9700
N3—C8	1.389 (10)	C7—C8	1.445 (11)
N4—C9	1.359 (11)	C7—H7	0.9300
N4—C10	1.364 (11)	C8—C9	1.350 (11)
N4—H4A	0.8600	C10—H10	0.9300
N2—Ni1—N1	79.7 (3)	N1—C1—H1	117.9
N2—Ni1—O1	91.5 (3)	C2—C1—H1	117.9
N1—Ni1—O1	87.5 (3)	C3—C2—C1	118.0 (9)
N2—Ni1—N3	79.4 (3)	C3—C2—H2	121.0
N1—Ni1—N3	158.8 (3)	C1—C2—H2	121.0
O1—Ni1—N3	89.4 (3)	C2—C3—C4	119.7 (9)
N2—Ni1—Br1^i	177.93 (19)	C2—C3—H3	120.1
N1—Ni1—Br1^i	102.3 (2)	C4—C3—H3	120.1
O1—Ni1—Br1^i	88.53 (16)	C5—C4—C3	118.7 (8)
N3—Ni1—Br1^i	98.55 (18)	C5—C4—H4	120.7
N2—Ni1—Br1	92.0 (2)	C3—C4—H4	120.7
N1—Ni1—Br1	90.9 (2)	N1—C5—C4	122.8 (8)
O1—Ni1—Br1	175.78 (18)	N1—C5—C6	117.1 (7)
N3—Ni1—Br1	93.5 (2)	C4—C5—C6	120.0 (7)
Br1^i—Ni1—Br1	88.01 (5)	N2—C6—C5	109.5 (7)
Ni1^i—Br1—Ni1	91.99 (5)	N2—C6—H6A	109.8
C1—N1—C5	116.6 (7)	C5—C6—H6A	109.8
C1—N1—Ni1	127.7 (6)	N2—C6—H6B	109.8
C5—N1—Ni1	115.7 (6)	C5—C6—H6B	109.8
C7—N2—C6	124.2 (7)	H6A—C6—H6B	108.2
C7—N2—Ni1	117.7 (5)	N2—C7—C8	116.5 (7)
C6—N2—Ni1	117.9 (5)	N2—C7—H7	121.7
C10—N3—C8	105.8 (7)	C8—C7—H7	121.7
C10—N3—Ni1	144.4 (6)	C9—C8—N3	109.1 (7)
C8—N3—Ni1	109.7 (5)	C9—C8—C7	134.2 (8)
C9—N4—C10	106.7 (7)	N3—C8—C7	116.6 (7)
C9—N4—H4A	126.6	C8—C9—N4	106.7 (8)
C10—N4—H4A	126.6	C8—C9—Br2	131.7 (7)
Ni1—O1—H1W	124.8	N4—C9—Br2	121.6 (7)
Ni1—O1—H2W	129.4	N3—C10—N4	111.5 (8)
H1W—O1—H2W	96.9	N3—C10—H10	124.2
N1—C1—C2	124.1 (9)	N4—C10—H10	124.2
N2—Ni1—Br1—Ni1^i	177.93 (19)	C5—N1—C1—C2	0.5 (15)
N1—Ni1—Br1—Ni1^i	−102.3 (2)	Ni1—N1—C1—C2	179.2 (8)
N3—Ni1—Br1—Ni1^i	98.45 (18)	N1—C1—C2—C3	−1.5 (17)
Br1^i—Ni1—Br1—Ni1^i	0.0	C1—C2—C3—C4	1.3 (17)
N2—Ni1—N1—C1	−177.1 (9)	C2—C3—C4—C5	−0.3 (17)
O1—Ni1—N1—C1	−85.1 (8)	C1—N1—C5—C4	0.6 (14)
N3—Ni1—N1—C1	−166.8 (8)	Ni1—N1—C5—C4	−178.2 (7)
Br1^i—Ni1—N1—C1	2.8 (9)	C1—N1—C5—C6	178.1 (9)
Br1—Ni1—N1—C1	91.0 (8)	Ni1—N1—C5—C6	−0.7 (11)
N2—Ni1—N1—C5	1.5 (6)	C3—C4—C5—N1	−0.7 (15)
O1—Ni1—N1—C5	93.6 (6)	C3—C4—C5—C6	−178.2 (10)
N3—Ni1—N1—C5	11.9 (12)	C7—N2—C6—C5	−174.0 (9)
Br1^i—Ni1—N1—C5	−178.5 (6)	Ni1—N2—C6—C5	2.4 (11)
Br1—Ni1—N1—C5	−90.3 (6)	N1—C5—C6—N2	−1.0 (13)
N1—Ni1—N2—C7	174.4 (7)	C4—C5—C6—N2	176.6 (9)
O1—Ni1—N2—C7	87.3 (7)	C6—N2—C7—C8	177.1 (8)
N3—Ni1—N2—C7	−1.8 (7)	Ni1—N2—C7—C8	0.7 (11)
Br1—Ni1—N2—C7	−95.0 (7)	C10—N3—C8—C9	0.5 (11)
N1—Ni1—N2—C6	−2.2 (7)	Ni1—N3—C8—C9	178.9 (6)
O1—Ni1—N2—C6	−89.3 (7)	C10—N3—C8—C7	178.7 (8)
N3—Ni1—N2—C6	−178.4 (8)	Ni1—N3—C8—C7	−2.9 (10)
Br1—Ni1—N2—C6	88.4 (7)	N2—C7—C8—C9	179.2 (10)
N2—Ni1—N3—C10	179.7 (12)	N2—C7—C8—N3	1.6 (12)
N1—Ni1—N3—C10	169.4 (10)	N3—C8—C9—N4	−2.0 (11)
O1—Ni1—N3—C10	88.1 (12)	C7—C8—C9—N4	−179.7 (10)
Br1^i—Ni1—N3—C10	−0.3 (12)	N3—C8—C9—Br2	−180.0 (7)
Br1—Ni1—N3—C10	−88.9 (12)	C7—C8—C9—Br2	2.3 (17)
N2—Ni1—N3—C8	2.4 (6)	C10—N4—C9—C8	2.6 (11)
N1—Ni1—N3—C8	−7.9 (12)	C10—N4—C9—Br2	−179.2 (7)
O1—Ni1—N3—C8	−89.3 (6)	C8—N3—C10—N4	1.1 (11)
Br1^i—Ni1—N3—C8	−177.7 (6)	Ni1—N3—C10—N4	−176.2 (8)
Br1—Ni1—N3—C8	93.8 (6)	C9—N4—C10—N3	−2.4 (12)

Symmetry code: (i) −x, −y, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1W···Br3	0.80	2.54	3.306 (6)	161
O1—H2W···Br3^ii	0.87	2.46	3.315 (6)	168
N4—H4A···Br3^iii	0.86	2.43	3.266 (7)	165

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