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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 NiII 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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680603532X/wn2067sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680603532X/wn2067Isup2.hkl
Contains datablock I

CCDC reference: 625019

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 top

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 top
Crystal data top
[Ni2Br2(C10H9BrN4)2(H2O)2]Br2Z = 1
Mr = 1003.24F(000) = 480
Triclinic, P1Dx = 2.207 Mg m3
Hall symbol: -P 1Melting point: 506 K
a = 8.4833 (17) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.4187 (19) ÅCell parameters from 25 reflections
c = 10.748 (2) Åθ = 16.9–26.8°
α = 90.16 (3)°µ = 9.22 mm1
β = 107.77 (3)°T = 298 K
γ = 111.40 (3)°Prism, green
V = 755.1 (3) Å30.2 × 0.15 × 0.15 mm
Data collection top
Rigaku AFC-7S
diffractometer
1603 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.039
Graphite monochromatorθmax = 26.0°, θmin = 2.0°
ω/2θ scansh = 100
Absorption correction: ψ scan
(North et al., 1968)
k = 1011
Tmin = 0.196, Tmax = 0.252l = 1213
3189 measured reflections3 standard reflections every 150 reflections
2977 independent reflections intensity decay: 0.5%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.128H-atom parameters constrained
S = 0.95 w = 1/[σ2(Fo2) + (0.0625P)2]
where P = (Fo2 + 2Fc2)/3
2977 reflections(Δ/σ)max < 0.001
172 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 0.85 e Å3
Special details top

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 (Å2) top
xyzUiso*/Ueq
Ni10.07931 (14)0.10344 (11)0.16618 (11)0.0342 (3)
Br10.14088 (12)0.15998 (9)0.05372 (9)0.0402 (2)
Br20.82620 (14)0.26096 (13)0.48128 (11)0.0638 (3)
Br30.28619 (13)0.27035 (10)0.61345 (10)0.0490 (3)
N10.0806 (9)0.2305 (8)0.1323 (7)0.0430 (18)
N20.2629 (9)0.3116 (7)0.2584 (7)0.0376 (16)
N30.3064 (9)0.0500 (7)0.2466 (7)0.0412 (18)
N40.5402 (10)0.0093 (9)0.3369 (8)0.054 (2)
H4A0.60390.06400.35950.065*
O10.0103 (9)0.0483 (6)0.3350 (6)0.0567 (18)
H1W0.07620.08180.40880.068*
H2W0.05340.03970.35250.068*
C10.2567 (12)0.1804 (10)0.0714 (10)0.050 (2)
H10.31800.07670.03840.060*
C20.3540 (14)0.2724 (11)0.0541 (10)0.057 (3)
H20.47670.23260.00910.069*
C30.2648 (13)0.4242 (12)0.1052 (12)0.063 (3)
H30.32710.48890.09680.076*
C40.0827 (14)0.4807 (10)0.1690 (10)0.057 (3)
H40.02020.58370.20380.068*
C50.0050 (11)0.3820 (8)0.1802 (8)0.038 (2)
C60.2041 (13)0.4392 (10)0.2533 (12)0.062 (3)
H6A0.26840.51790.20880.074*
H6B0.22980.48440.34210.074*
C70.4182 (12)0.3208 (9)0.3217 (8)0.039 (2)
H70.50830.41330.36690.047*
C80.4498 (11)0.1802 (9)0.3204 (8)0.039 (2)
C90.5940 (12)0.1437 (10)0.3735 (9)0.044 (2)
C100.3656 (13)0.0594 (10)0.2575 (10)0.052 (3)
H100.29770.15970.21640.063*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0337 (6)0.0239 (5)0.0423 (7)0.0100 (4)0.0099 (5)0.0007 (4)
Br10.0400 (5)0.0273 (4)0.0482 (6)0.0074 (4)0.0141 (4)0.0019 (4)
Br20.0407 (6)0.0775 (7)0.0636 (7)0.0247 (5)0.0017 (5)0.0045 (6)
Br30.0479 (6)0.0316 (5)0.0591 (6)0.0095 (4)0.0135 (5)0.0039 (4)
N10.039 (4)0.039 (4)0.051 (5)0.015 (3)0.015 (4)0.004 (3)
N20.030 (4)0.030 (3)0.046 (4)0.010 (3)0.005 (3)0.004 (3)
N30.033 (4)0.034 (4)0.054 (5)0.012 (3)0.012 (4)0.002 (3)
N40.052 (5)0.047 (4)0.064 (6)0.029 (4)0.009 (4)0.004 (4)
O10.066 (4)0.039 (3)0.046 (4)0.005 (3)0.022 (3)0.000 (3)
C10.043 (6)0.038 (5)0.066 (7)0.015 (4)0.016 (5)0.002 (4)
C20.045 (6)0.055 (6)0.070 (7)0.024 (5)0.009 (5)0.003 (5)
C30.043 (6)0.056 (6)0.095 (9)0.029 (5)0.014 (6)0.009 (6)
C40.073 (7)0.029 (5)0.075 (7)0.029 (5)0.024 (6)0.005 (5)
C50.038 (5)0.022 (4)0.050 (6)0.009 (4)0.014 (4)0.003 (4)
C60.050 (6)0.026 (4)0.100 (9)0.015 (4)0.012 (6)0.000 (5)
C70.040 (5)0.024 (4)0.043 (5)0.005 (4)0.009 (4)0.004 (4)
C80.033 (4)0.043 (5)0.033 (5)0.014 (4)0.000 (4)0.002 (4)
C90.043 (5)0.047 (5)0.045 (6)0.020 (4)0.015 (4)0.005 (4)
C100.057 (6)0.032 (5)0.062 (6)0.016 (4)0.013 (5)0.000 (4)
Geometric parameters (Å, º) top
Ni1—N22.017 (6)O1—H1W0.8006
Ni1—N12.071 (7)O1—H2W0.8662
Ni1—O12.082 (6)C1—C21.377 (13)
Ni1—N32.099 (7)C1—H10.9300
Ni1—Br1i2.5157 (17)C2—C31.367 (13)
Ni1—Br12.5884 (16)C2—H20.9300
Br1—Ni1i2.5157 (17)C3—C41.376 (13)
Br2—C91.858 (9)C3—H30.9300
N1—C11.331 (11)C4—C51.372 (11)
N1—C51.356 (10)C4—H40.9300
N2—C71.255 (10)C5—C61.511 (12)
N2—C61.456 (10)C6—H6A0.9700
N3—C101.292 (10)C6—H6B0.9700
N3—C81.389 (10)C7—C81.445 (11)
N4—C91.359 (11)C7—H70.9300
N4—C101.364 (11)C8—C91.350 (11)
N4—H4A0.8600C10—H100.9300
N2—Ni1—N179.7 (3)N1—C1—H1117.9
N2—Ni1—O191.5 (3)C2—C1—H1117.9
N1—Ni1—O187.5 (3)C3—C2—C1118.0 (9)
N2—Ni1—N379.4 (3)C3—C2—H2121.0
N1—Ni1—N3158.8 (3)C1—C2—H2121.0
O1—Ni1—N389.4 (3)C2—C3—C4119.7 (9)
N2—Ni1—Br1i177.93 (19)C2—C3—H3120.1
N1—Ni1—Br1i102.3 (2)C4—C3—H3120.1
O1—Ni1—Br1i88.53 (16)C5—C4—C3118.7 (8)
N3—Ni1—Br1i98.55 (18)C5—C4—H4120.7
N2—Ni1—Br192.0 (2)C3—C4—H4120.7
N1—Ni1—Br190.9 (2)N1—C5—C4122.8 (8)
O1—Ni1—Br1175.78 (18)N1—C5—C6117.1 (7)
N3—Ni1—Br193.5 (2)C4—C5—C6120.0 (7)
Br1i—Ni1—Br188.01 (5)N2—C6—C5109.5 (7)
Ni1i—Br1—Ni191.99 (5)N2—C6—H6A109.8
C1—N1—C5116.6 (7)C5—C6—H6A109.8
C1—N1—Ni1127.7 (6)N2—C6—H6B109.8
C5—N1—Ni1115.7 (6)C5—C6—H6B109.8
C7—N2—C6124.2 (7)H6A—C6—H6B108.2
C7—N2—Ni1117.7 (5)N2—C7—C8116.5 (7)
C6—N2—Ni1117.9 (5)N2—C7—H7121.7
C10—N3—C8105.8 (7)C8—C7—H7121.7
C10—N3—Ni1144.4 (6)C9—C8—N3109.1 (7)
C8—N3—Ni1109.7 (5)C9—C8—C7134.2 (8)
C9—N4—C10106.7 (7)N3—C8—C7116.6 (7)
C9—N4—H4A126.6C8—C9—N4106.7 (8)
C10—N4—H4A126.6C8—C9—Br2131.7 (7)
Ni1—O1—H1W124.8N4—C9—Br2121.6 (7)
Ni1—O1—H2W129.4N3—C10—N4111.5 (8)
H1W—O1—H2W96.9N3—C10—H10124.2
N1—C1—C2124.1 (9)N4—C10—H10124.2
N2—Ni1—Br1—Ni1i177.93 (19)C5—N1—C1—C20.5 (15)
N1—Ni1—Br1—Ni1i102.3 (2)Ni1—N1—C1—C2179.2 (8)
N3—Ni1—Br1—Ni1i98.45 (18)N1—C1—C2—C31.5 (17)
Br1i—Ni1—Br1—Ni1i0.0C1—C2—C3—C41.3 (17)
N2—Ni1—N1—C1177.1 (9)C2—C3—C4—C50.3 (17)
O1—Ni1—N1—C185.1 (8)C1—N1—C5—C40.6 (14)
N3—Ni1—N1—C1166.8 (8)Ni1—N1—C5—C4178.2 (7)
Br1i—Ni1—N1—C12.8 (9)C1—N1—C5—C6178.1 (9)
Br1—Ni1—N1—C191.0 (8)Ni1—N1—C5—C60.7 (11)
N2—Ni1—N1—C51.5 (6)C3—C4—C5—N10.7 (15)
O1—Ni1—N1—C593.6 (6)C3—C4—C5—C6178.2 (10)
N3—Ni1—N1—C511.9 (12)C7—N2—C6—C5174.0 (9)
Br1i—Ni1—N1—C5178.5 (6)Ni1—N2—C6—C52.4 (11)
Br1—Ni1—N1—C590.3 (6)N1—C5—C6—N21.0 (13)
N1—Ni1—N2—C7174.4 (7)C4—C5—C6—N2176.6 (9)
O1—Ni1—N2—C787.3 (7)C6—N2—C7—C8177.1 (8)
N3—Ni1—N2—C71.8 (7)Ni1—N2—C7—C80.7 (11)
Br1—Ni1—N2—C795.0 (7)C10—N3—C8—C90.5 (11)
N1—Ni1—N2—C62.2 (7)Ni1—N3—C8—C9178.9 (6)
O1—Ni1—N2—C689.3 (7)C10—N3—C8—C7178.7 (8)
N3—Ni1—N2—C6178.4 (8)Ni1—N3—C8—C72.9 (10)
Br1—Ni1—N2—C688.4 (7)N2—C7—C8—C9179.2 (10)
N2—Ni1—N3—C10179.7 (12)N2—C7—C8—N31.6 (12)
N1—Ni1—N3—C10169.4 (10)N3—C8—C9—N42.0 (11)
O1—Ni1—N3—C1088.1 (12)C7—C8—C9—N4179.7 (10)
Br1i—Ni1—N3—C100.3 (12)N3—C8—C9—Br2180.0 (7)
Br1—Ni1—N3—C1088.9 (12)C7—C8—C9—Br22.3 (17)
N2—Ni1—N3—C82.4 (6)C10—N4—C9—C82.6 (11)
N1—Ni1—N3—C87.9 (12)C10—N4—C9—Br2179.2 (7)
O1—Ni1—N3—C889.3 (6)C8—N3—C10—N41.1 (11)
Br1i—Ni1—N3—C8177.7 (6)Ni1—N3—C10—N4176.2 (8)
Br1—Ni1—N3—C893.8 (6)C9—N4—C10—N32.4 (12)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1W···Br30.802.543.306 (6)161
O1—H2W···Br3ii0.872.463.315 (6)168
N4—H4A···Br3iii0.862.433.266 (7)165
Symmetry codes: (ii) x, y, z+1; (iii) x+1, y, z+1.
 

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