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In the title complex, [Ni(C16H22N6)2]Br2, the Ni atom is in a slightly distorted octa­hedral coordination environment, having crystallographic 2/m symmetry. The Ni atom is coordinated by the six pyrazol­yl rings of the two tridentate tris­(3,5-dimethyl­pyrazol­yl)methane ligands, with Ni-N distances in the range 2.0753 (17)-2.110 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805009451/lh6391sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805009451/lh6391Isup2.hkl
Contains datablock I

CCDC reference: 270489

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.040
  • wR factor = 0.108
  • Data-to-parameter ratio = 15.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.31 Ratio
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.124 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.81 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.46 Ratio
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 5 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 5 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

Bis[tris(3,5-dimethylpyrazolyl)methane]nickel(II) dibromide top
Crystal data top
[Ni(C16H22N6)2]Br2F(000) = 836.0
Mr = 815.32Dx = 1.467 Mg m3
Monoclinic, C2/mCu Kα radiation, λ = 1.54178 Å
Hall symbol: -C 2yCell parameters from 8952 reflections
a = 18.9240 (2) Åθ = 4.7–72.9°
b = 10.996 (1) ŵ = 3.61 mm1
c = 8.8821 (1) ÅT = 298 K
β = 92.580 (1)°Block, translucent pale pink
V = 1846.39 (17) Å30.18 × 0.15 × 0.10 mm
Z = 2
Data collection top
Bruker SMART 2K/Platform
diffractometer
1907 independent reflections
Radiation source: normal-focus xray tube1702 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.125
Detector resolution: 5.5 pixels mm-1θmax = 72.9°, θmin = 4.7°
ω scansh = 2323
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 1313
Tmin = 0.447, Tmax = 0.697l = 1010
11178 measured reflections
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)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0739P)2]
where P = (Fo2 + 2Fc2)/3
1907 reflections(Δ/σ)max = 0.001
126 parametersΔρmax = 0.60 e Å3
0 restraintsΔρmin = 0.60 e Å3
Special details top

Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a glass fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis.

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. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factor_obs 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*/UeqOcc. (<1)
Ni0.00000.00000.00000.0274 (2)
C110.14287 (14)0.00000.1496 (3)0.0292 (6)
H110.18820.00000.19890.035*
N10.10228 (14)0.00000.1050 (3)0.0399 (6)
N20.15766 (13)0.00000.0105 (3)0.0348 (5)
C10.0871 (3)0.00000.3796 (5)0.101 (2)
H1A0.10900.05100.45600.151*0.50
H1B0.04070.03050.35280.151*0.50
H1C0.08340.08150.41730.151*0.50
C20.1312 (2)0.00000.2423 (4)0.0543 (9)
C30.2049 (2)0.00000.2390 (5)0.0556 (10)
H30.23680.00000.32160.067*
C40.22085 (17)0.00000.0905 (4)0.0471 (8)
C50.2907 (2)0.00000.0190 (6)0.0821 (16)
H5A0.28580.03720.07870.123*0.50
H5B0.32440.04500.08100.123*0.50
H5C0.30690.08220.00870.123*0.50
N30.03823 (9)0.12830 (17)0.1472 (2)0.0406 (5)
N40.10484 (9)0.10856 (15)0.1964 (2)0.0325 (4)
C60.05222 (19)0.2906 (3)0.1803 (5)0.0876 (13)
H6A0.08580.22720.16310.131*
H6B0.06750.33650.26780.131*
H6C0.04880.34340.09420.131*
C70.01861 (14)0.2355 (2)0.2051 (3)0.0522 (7)
C80.07280 (15)0.2840 (2)0.2889 (3)0.0551 (7)
H80.07190.35770.34030.066*
C90.12695 (13)0.2030 (2)0.2809 (3)0.0418 (5)
C100.19805 (15)0.2092 (3)0.3439 (4)0.0619 (8)
H10A0.23320.21810.26320.093*
H10B0.20020.27760.41060.093*
H10C0.20690.13580.39860.093*
Br0.658821 (18)0.00000.43123 (4)0.04606 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0262 (3)0.0287 (4)0.0276 (4)0.0000.0030 (3)0.000
C110.0262 (12)0.0271 (13)0.0347 (15)0.0000.0055 (11)0.000
N10.0322 (12)0.0594 (17)0.0282 (13)0.0000.0007 (10)0.000
N20.0272 (11)0.0412 (14)0.0362 (14)0.0000.0024 (10)0.000
C10.065 (3)0.208 (8)0.030 (2)0.0000.000 (2)0.000
C20.0479 (19)0.080 (3)0.0346 (19)0.0000.0067 (15)0.000
C30.0433 (19)0.076 (3)0.046 (2)0.0000.0167 (16)0.000
C40.0313 (16)0.057 (2)0.053 (2)0.0000.0064 (15)0.000
C50.0297 (18)0.137 (5)0.080 (3)0.0000.0007 (19)0.000
N30.0323 (9)0.0387 (10)0.0520 (11)0.0088 (7)0.0130 (8)0.0159 (8)
N40.0320 (8)0.0282 (9)0.0379 (9)0.0027 (7)0.0094 (7)0.0042 (6)
C60.0598 (18)0.073 (2)0.133 (3)0.0354 (17)0.036 (2)0.058 (2)
C70.0464 (13)0.0438 (13)0.0675 (17)0.0141 (11)0.0157 (12)0.0229 (12)
C80.0623 (16)0.0368 (12)0.0678 (17)0.0093 (11)0.0215 (14)0.0211 (11)
C90.0490 (13)0.0311 (11)0.0466 (13)0.0010 (9)0.0147 (10)0.0050 (9)
C100.0597 (16)0.0404 (13)0.089 (2)0.0018 (12)0.0369 (16)0.0177 (13)
Br0.0467 (2)0.0402 (2)0.0506 (3)0.0000.00569 (16)0.000
Geometric parameters (Å, º) top
Ni—N3i2.0753 (17)C3—H30.9300
Ni—N32.0754 (17)C4—C51.493 (5)
Ni—N3ii2.0754 (17)C5—H5A0.9600
Ni—N3iii2.0754 (17)C5—H5B0.9600
Ni—N12.110 (3)C5—H5C0.9600
Ni—N1iii2.110 (3)N3—C71.332 (3)
C11—N21.438 (4)N3—N41.370 (2)
C11—N41.445 (2)N4—C91.358 (3)
C11—N4i1.445 (2)C6—C71.496 (4)
C11—H110.9800C6—H6A0.9600
N1—C21.314 (4)C6—H6B0.9600
N1—N21.372 (3)C6—H6C0.9600
N2—C41.363 (4)C7—C81.399 (3)
C1—C21.509 (6)C8—C91.357 (3)
C1—H1A0.9600C8—H80.9300
C1—H1B0.9600C9—C101.482 (3)
C1—H1C0.9600C10—H10A0.9600
C2—C31.395 (5)C10—H10B0.9600
C3—C41.366 (5)C10—H10C0.9600
N3i—Ni—N385.65 (11)C2—C3—H3126.7
N3i—Ni—N3ii180.0N2—C4—C3106.0 (3)
N3—Ni—N3ii94.35 (11)N2—C4—C5123.5 (3)
N3i—Ni—N3iii94.35 (11)C3—C4—C5130.5 (3)
N3—Ni—N3iii180.0C4—C5—H5A109.5
N3ii—Ni—N3iii85.65 (11)C4—C5—H5B109.5
N3i—Ni—N186.53 (7)H5A—C5—H5B109.5
N3—Ni—N186.53 (7)C4—C5—H5C109.5
N3ii—Ni—N193.47 (7)H5A—C5—H5C109.5
N3iii—Ni—N193.47 (7)H5B—C5—H5C109.5
N3i—Ni—N1iii93.47 (7)C7—N3—N4105.14 (17)
N3—Ni—N1iii93.47 (7)C7—N3—Ni138.22 (16)
N3ii—Ni—N1iii86.53 (7)N4—N3—Ni116.45 (12)
N3iii—Ni—N1iii86.53 (7)C9—N4—N3111.48 (17)
N1—Ni—N1iii180.0C9—N4—C11128.95 (19)
N2—C11—N4110.91 (15)N3—N4—C11119.49 (17)
N2—C11—N4i110.91 (15)C7—C6—H6A109.5
N4—C11—N4i111.4 (2)C7—C6—H6B109.5
N2—C11—H11107.8H6A—C6—H6B109.5
N4—C11—H11107.8C7—C6—H6C109.5
N4i—C11—H11107.8H6A—C6—H6C109.5
C2—N1—N2105.6 (3)H6B—C6—H6C109.5
C2—N1—Ni138.2 (2)N3—C7—C8110.1 (2)
N2—N1—Ni116.14 (19)N3—C7—C6122.5 (2)
C4—N2—N1111.0 (3)C8—C7—C6127.4 (2)
C4—N2—C11130.0 (3)C9—C8—C7107.0 (2)
N1—N2—C11119.0 (2)C9—C8—H8126.5
C2—C1—H1A109.5C7—C8—H8126.5
C2—C1—H1B109.5C8—C9—N4106.3 (2)
H1A—C1—H1B109.5C8—C9—C10130.3 (2)
C2—C1—H1C109.5N4—C9—C10123.5 (2)
H1A—C1—H1C109.5C9—C10—H10A109.5
H1B—C1—H1C109.5C9—C10—H10B109.5
N1—C2—C3110.8 (3)H10A—C10—H10B109.5
N1—C2—C1121.8 (3)C9—C10—H10C109.5
C3—C2—C1127.4 (4)H10A—C10—H10C109.5
C4—C3—C2106.5 (3)H10B—C10—H10C109.5
C4—C3—H3126.7
N3i—Ni—N1—C2137.08 (6)C2—C3—C4—N20.0
N3—Ni—N1—C2137.08 (6)C2—C3—C4—C5180.0
N3ii—Ni—N1—C242.92 (6)N1—Ni—N3—C7132.5 (3)
N3iii—Ni—N1—C242.92 (6)N1iii—Ni—N3—C747.5 (3)
N3i—Ni—N1—N242.92 (6)N1—Ni—N3—N441.38 (16)
N3—Ni—N1—N242.92 (6)N1iii—Ni—N3—N4138.62 (16)
N3ii—Ni—N1—N2137.08 (6)C7—N3—N4—C91.3 (3)
N3iii—Ni—N1—N2137.08 (6)Ni—N3—N4—C9174.53 (16)
C2—N1—N2—C40.0C7—N3—N4—C11178.2 (2)
Ni—N1—N2—C4180.0Ni—N3—N4—C112.4 (3)
C2—N1—N2—C11180.0N2—C11—N4—C9111.9 (3)
Ni—N1—N2—C110.0N4i—C11—N4—C9124.0 (2)
N4—C11—N2—C4117.85 (16)N2—C11—N4—N364.4 (3)
N4i—C11—N2—C4117.85 (16)N4i—C11—N4—N359.6 (3)
N4—C11—N2—N162.15 (16)N4—N3—C7—C80.7 (3)
N4i—C11—N2—N162.15 (16)Ni—N3—C7—C8173.6 (2)
N2—N1—C2—C30.0N4—N3—C7—C6178.9 (3)
Ni—N1—C2—C3180.0Ni—N3—C7—C66.7 (5)
N2—N1—C2—C1180.0N3—C7—C8—C90.1 (4)
Ni—N1—C2—C10.0C6—C7—C8—C9179.7 (4)
N1—C2—C3—C40.0C7—C8—C9—N40.8 (3)
C1—C2—C3—C4180.0C7—C8—C9—C10177.7 (3)
N1—N2—C4—C30.0N3—N4—C9—C81.3 (3)
C11—N2—C4—C3180.0C11—N4—C9—C8177.9 (2)
N1—N2—C4—C5180.0N3—N4—C9—C10177.3 (2)
C11—N2—C4—C50.0C11—N4—C9—C100.7 (4)
Symmetry codes: (i) x, y, z; (ii) x, y, z; (iii) x, y, z.
 

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