Literature DB >> 24109278

Bis[μ-3,5-bis-(pyridin-2-yl)pyrazolato]bis-[(hexa-fluoro-phosphato)copper(II)].

Akio Mishima1, Nagisa Katsuta, Midori Furusyou, Akira Fuyuhiro, Satoshi Kawata.   

Abstract

The title dinuclear complex mol-ecule, [Cu2(C13H9N4)2(PF6)2], lies about an inversion center. The Cu(II) atom shows a square-pyramidal coordination geometry with the basal plane formed by four N atoms of the two bis-chelating 3,5-bis-(pyridin-2-yl)pyrazolate ions and with one F atom of the hexa-fluoro-phosphate ion in the apical position. Mol-ecules are stacked in a column along the a axis through C-H⋯F hydrogen bonds. The columns are further linked by other C-H⋯F hydrogen bonds, forming a three-dimensional network.

Entities:  

Year:  2013        PMID： 24109278      PMCID： PMC3793691          DOI： 10.1107/S1600536813018813

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For metal complexes of 3,5-bis­(2-pyrid­yl)pyrazole, see: Klingele et al. (2009 ▶); Yoneda, Adachi, Hayami et al. (2006 ▶); Yoneda, Adachi, Nishio et al. (2006 ▶); Ishikawa et al. (2010 ▶); Mishima et al. (2011 ▶); Washizaki et al. (2012 ▶). For an example of a coordinated hexa­fluoro­phosphate ion, see: Noro et al. (2011 ▶).

Experimental

Crystal data

[Cu2(C13H9N4)2(F6P)2] M = 859.52 Monoclinic, a = 6.3558 (4) Å b = 21.2388 (14) Å c = 10.9252 (9) Å β = 95.753 (2)° V = 1467.36 (18) Å3 Z = 2 Mo Kα radiation μ = 1.67 mm−1 T = 200 K 0.50 × 0.15 × 0.10 mm

Data collection

Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.603, T max = 0.845 23498 measured reflections 3364 independent reflections 3035 reflections with F 2 > 2σ(F 2) R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 0.074 S = 1.05 3364 reflections 226 parameters H-atom parameters constrained Δρmax = 0.44 e Å−3 Δρmin = −0.19 e Å−3 Data collection: RAPID-AUTO (Rigaku, 2002 ▶); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: Il Milione (Burla et al., 2007 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: CrystalStructure (Rigaku, 2010 ▶); software used to prepare material for publication: CrystalStructure. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536813018813/is5289sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813018813/is5289Isup2.hkl Click here for additional data file. Supplementary material file. DOI: 10.1107/S1600536813018813/is5289Isup3.cdx Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cu2(C13H9N4)2(F6P)2]F(000) = 852.00
Mr = 859.52Dx = 1.945 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ybcCell parameters from 17353 reflections
a = 6.3558 (4) Åθ = 3.2–27.5°
b = 21.2388 (14) ŵ = 1.67 mm−1
c = 10.9252 (9) ÅT = 200 K
β = 95.753 (2)°Block, purple
V = 1467.36 (18) Å30.50 × 0.15 × 0.10 mm
Z = 2
Rigaku R-AXIS RAPID diffractometer3035 reflections with F2 > 2σ(F2)
Detector resolution: 10.000 pixels mm-1Rint = 0.028
¥w scansθmax = 27.5°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)h = −7→8
Tmin = 0.603, Tmax = 0.845k = −27→27
23498 measured reflectionsl = −14→14
3364 independent reflections
Refinement on F2Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.074H-atom parameters constrained
S = 1.05w = 1/[σ2(Fo2) + (0.0407P)2 + 0.8933P] where P = (Fo2 + 2Fc2)/3
3364 reflections(Δ/σ)max = 0.005
226 parametersΔρmax = 0.44 e Å−3
0 restraintsΔρmin = −0.19 e Å−3
Primary atom site location: structure-invariant direct methods
Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 sigma(F2) is used only for calculating R-factor (gt).
xyzUiso*/Ueq
Cu10.24888 (3)1.033789 (9)0.417882 (19)0.02189 (8)
P10.03196 (7)1.13684 (2)0.14887 (5)0.02699 (12)
F10.0266 (2)1.09594 (7)0.27373 (13)0.0462 (4)
F20.28337 (18)1.14060 (7)0.17046 (13)0.0442 (4)
F3−0.22096 (18)1.13202 (6)0.13015 (12)0.0396 (3)
F40.0145 (3)1.19979 (7)0.22615 (15)0.0542 (4)
F50.0487 (3)1.07334 (7)0.07324 (15)0.0563 (4)
F60.0329 (3)1.17709 (8)0.02601 (13)0.0538 (4)
N1−0.4133 (3)0.88408 (7)0.53595 (15)0.0270 (4)
N2−0.0897 (3)0.93626 (7)0.45127 (14)0.0253 (3)
N30.0774 (3)0.95817 (7)0.39846 (15)0.0252 (3)
N40.4018 (3)0.98801 (7)0.28636 (15)0.0267 (4)
C1−0.5796 (4)0.85849 (11)0.5849 (2)0.0407 (5)
C2−0.6626 (4)0.80010 (12)0.5503 (3)0.0457 (6)
C3−0.5719 (4)0.76610 (11)0.4628 (3)0.0422 (5)
C4−0.4009 (4)0.79120 (10)0.4109 (2)0.0361 (5)
C5−0.3257 (3)0.85002 (9)0.44940 (18)0.0267 (4)
C6−0.1453 (3)0.88030 (9)0.40028 (18)0.0270 (4)
C7−0.0116 (3)0.86473 (9)0.31120 (19)0.0308 (4)
C80.1266 (3)0.91584 (9)0.31413 (17)0.0267 (4)
C90.3078 (3)0.93294 (9)0.24875 (17)0.0259 (4)
C100.3792 (4)0.89636 (10)0.15631 (19)0.0345 (5)
C110.5527 (4)0.91622 (11)0.1003 (2)0.0379 (5)
C120.6503 (4)0.97141 (10)0.1374 (3)0.0394 (5)
C130.5705 (4)1.00590 (10)0.2299 (3)0.0395 (5)
H1−0.64290.88150.64610.0489*
H2−0.78090.78390.58680.0549*
H3−0.62580.72580.43810.0506*
H4−0.33600.76850.34980.0433*
H5−0.01400.82820.26080.0370*
H60.30960.85810.13190.0413*
H70.60390.89190.03660.0454*
H80.77050.98580.10050.0473*
H90.63861.04430.25470.0474*
U11U22U33U12U13U23
Cu10.02108 (12)0.02079 (12)0.02492 (13)−0.00163 (8)0.00777 (8)0.00105 (8)
P10.0235 (3)0.0286 (3)0.0298 (3)0.00159 (18)0.00704 (18)0.00549 (18)
F10.0339 (7)0.0609 (9)0.0441 (8)0.0039 (6)0.0048 (6)0.0282 (7)
F20.0238 (6)0.0595 (9)0.0501 (8)−0.0005 (6)0.0075 (5)0.0071 (7)
F30.0243 (6)0.0452 (7)0.0494 (8)0.0015 (5)0.0050 (5)0.0164 (6)
F40.0554 (9)0.0404 (8)0.0704 (10)−0.0047 (7)0.0235 (8)−0.0159 (7)
F50.0550 (9)0.0471 (8)0.0710 (11)−0.0066 (7)0.0268 (8)−0.0213 (8)
F60.0451 (8)0.0709 (10)0.0458 (8)−0.0083 (7)0.0071 (6)0.0299 (7)
N10.0240 (7)0.0287 (8)0.0289 (8)−0.0056 (6)0.0053 (6)0.0000 (7)
N20.0256 (7)0.0233 (8)0.0282 (8)−0.0040 (6)0.0094 (6)−0.0015 (6)
N30.0246 (7)0.0246 (8)0.0279 (8)−0.0027 (6)0.0099 (6)−0.0008 (6)
N40.0275 (8)0.0237 (8)0.0307 (8)0.0021 (6)0.0118 (7)0.0025 (6)
C10.0360 (11)0.0469 (13)0.0420 (12)−0.0155 (10)0.0168 (9)−0.0086 (10)
C20.0388 (12)0.0486 (13)0.0521 (14)−0.0233 (11)0.0162 (10)−0.0052 (11)
C30.0375 (11)0.0326 (11)0.0567 (14)−0.0141 (9)0.0057 (10)−0.0042 (10)
C40.0332 (10)0.0275 (10)0.0486 (13)−0.0046 (8)0.0086 (9)−0.0067 (9)
C50.0220 (8)0.0260 (9)0.0324 (10)−0.0017 (7)0.0036 (7)0.0014 (8)
C60.0256 (9)0.0232 (9)0.0330 (10)−0.0025 (7)0.0069 (7)−0.0016 (7)
C70.0279 (9)0.0277 (10)0.0381 (11)−0.0038 (8)0.0095 (8)−0.0078 (8)
C80.0250 (8)0.0271 (9)0.0288 (9)−0.0005 (7)0.0073 (7)−0.0040 (7)
C90.0229 (8)0.0291 (9)0.0265 (9)0.0016 (7)0.0061 (7)0.0015 (7)
C100.0322 (10)0.0392 (11)0.0333 (10)−0.0023 (9)0.0100 (8)−0.0092 (9)
C110.0368 (11)0.0457 (12)0.0335 (11)0.0041 (10)0.0155 (9)−0.0042 (9)
C120.0369 (11)0.0407 (12)0.0449 (13)−0.0004 (9)0.0247 (10)0.0031 (9)
C130.0407 (12)0.0303 (10)0.0517 (13)−0.0069 (9)0.0257 (10)−0.0022 (9)
Cu1—F12.4027 (14)C3—C41.382 (4)
Cu1—N1i2.0698 (15)C4—C51.388 (3)
Cu1—N2i1.9393 (16)C5—C61.463 (3)
Cu1—N31.9405 (15)C6—C71.394 (3)
Cu1—N42.0577 (17)C7—C81.395 (3)
P1—F11.6205 (16)C8—C91.460 (3)
P1—F21.5937 (13)C9—C101.386 (3)
P1—F31.6033 (13)C10—C111.380 (4)
P1—F41.5911 (17)C11—C121.368 (4)
P1—F51.5908 (16)C12—C131.384 (4)
P1—F61.5919 (16)C1—H10.950
N1—C11.346 (3)C2—H20.950
N1—C51.354 (3)C3—H30.950
N2—N31.342 (3)C4—H40.950
N2—C61.345 (3)C7—H50.950
N3—C81.346 (3)C10—H60.950
N4—C91.358 (3)C11—H70.950
N4—C131.345 (3)C12—H80.950
C1—C21.385 (4)C13—H90.950
C2—C31.371 (4)
F1—Cu1—N1i86.91 (6)C1—C2—C3119.1 (3)
F1—Cu1—N2i89.26 (6)C2—C3—C4119.1 (3)
F1—Cu1—N395.51 (6)C3—C4—C5119.0 (2)
F1—Cu1—N495.15 (6)N1—C5—C4122.62 (18)
N1i—Cu1—N2i80.32 (7)N1—C5—C6114.45 (17)
N1i—Cu1—N3171.30 (7)C4—C5—C6122.94 (19)
N1i—Cu1—N4107.82 (7)N2—C6—C5114.80 (18)
N2i—Cu1—N391.34 (7)N2—C6—C7110.23 (17)
N2i—Cu1—N4170.90 (7)C5—C6—C7134.97 (18)
N3—Cu1—N480.32 (7)C6—C7—C8103.05 (17)
F1—P1—F290.45 (8)N3—C8—C7110.27 (17)
F1—P1—F388.14 (7)N3—C8—C9114.66 (17)
F1—P1—F489.73 (9)C7—C8—C9135.07 (19)
F1—P1—F589.48 (8)N4—C9—C8114.25 (17)
F1—P1—F6179.00 (8)N4—C9—C10122.46 (18)
F2—P1—F3178.59 (8)C8—C9—C10123.29 (18)
F2—P1—F490.10 (8)C9—C10—C11119.1 (2)
F2—P1—F590.07 (8)C10—C11—C12119.2 (3)
F2—P1—F690.55 (8)C11—C12—C13118.8 (3)
F3—P1—F489.93 (8)N4—C13—C12123.6 (2)
F3—P1—F589.88 (8)N1—C1—H1118.447
F3—P1—F690.86 (8)C2—C1—H1118.447
F4—P1—F5179.19 (9)C1—C2—H2120.455
F4—P1—F690.15 (9)C3—C2—H2120.458
F5—P1—F690.64 (9)C2—C3—H3120.463
Cu1—F1—P1141.77 (8)C4—C3—H3120.456
Cu1i—N1—C1129.86 (15)C3—C4—H4120.518
Cu1i—N1—C5112.79 (13)C5—C4—H4120.513
C1—N1—C5117.14 (17)C6—C7—H5128.470
Cu1i—N2—N3134.19 (12)C8—C7—H5128.475
Cu1i—N2—C6117.43 (13)C9—C10—H6120.440
N3—N2—C6108.34 (16)C11—C10—H6120.440
Cu1—N3—N2134.43 (13)C10—C11—H7120.375
Cu1—N3—C8117.46 (13)C12—C11—H7120.382
N2—N3—C8108.11 (15)C11—C12—H8120.612
Cu1—N4—C9113.20 (13)C13—C12—H8120.598
Cu1—N4—C13129.88 (14)N4—C13—H9118.220
C9—N4—C13116.83 (17)C12—C13—H9118.227
N1—C1—C2123.1 (3)
F1—Cu1—N1i—C1i−88.93 (13)Cu1i—N2—N3—C8177.44 (11)
F1—Cu1—N1i—C5i85.58 (10)Cu1i—N2—C6—C51.66 (19)
N1i—Cu1—F1—P165.41 (14)Cu1i—N2—C6—C7−177.98 (9)
F1—Cu1—N2i—N3i93.39 (14)N3—N2—C6—C5179.56 (13)
F1—Cu1—N2i—C6i−83.83 (10)N3—N2—C6—C7−0.08 (19)
N2i—Cu1—F1—P1145.75 (14)C6—N2—N3—Cu1179.64 (14)
F1—Cu1—N3—N2−87.27 (14)C6—N2—N3—C80.04 (18)
F1—Cu1—N3—C892.31 (11)Cu1—N3—C8—C7−179.67 (9)
N3—Cu1—F1—P1−122.97 (14)Cu1—N3—C8—C90.68 (19)
F1—Cu1—N4—C9−91.72 (10)N2—N3—C8—C70.02 (19)
F1—Cu1—N4—C1384.74 (13)N2—N3—C8—C9−179.64 (13)
N4—Cu1—F1—P1−42.23 (14)Cu1—N4—C9—C8−3.48 (18)
N1i—Cu1—N2i—N3i−179.62 (15)Cu1—N4—C9—C10176.67 (11)
N1i—Cu1—N2i—C6i3.16 (10)Cu1—N4—C13—C12−176.39 (12)
N2i—Cu1—N1i—C1i−178.70 (14)C9—N4—C13—C12−0.0 (3)
N2i—Cu1—N1i—C5i−4.20 (10)C13—N4—C9—C8179.56 (15)
N1i—Cu1—N4—C9179.88 (9)C13—N4—C9—C10−0.3 (3)
N1i—Cu1—N4—C13−3.67 (14)N1—C1—C2—C30.4 (4)
N4—Cu1—N1i—C1i5.49 (14)C1—C2—C3—C4−0.4 (4)
N4—Cu1—N1i—C5i180.00 (9)C2—C3—C4—C50.3 (3)
N2i—Cu1—N3—N22.12 (15)C3—C4—C5—N1−0.1 (3)
N2i—Cu1—N3—C8−178.30 (11)C3—C4—C5—C6179.75 (17)
N3—Cu1—N2i—N3i−2.11 (14)N1—C5—C6—N22.1 (3)
N3—Cu1—N2i—C6i−179.33 (11)N1—C5—C6—C7−178.41 (17)
N3—Cu1—N4—C93.01 (10)C4—C5—C6—N2−177.79 (17)
N3—Cu1—N4—C13179.47 (14)C4—C5—C6—C71.7 (4)
N4—Cu1—N3—N2178.43 (15)N2—C6—C7—C80.1 (2)
N4—Cu1—N3—C8−1.99 (10)C5—C6—C7—C8−179.44 (19)
F2—P1—F1—Cu1−17.33 (14)C6—C7—C8—N3−0.1 (2)
F3—P1—F1—Cu1162.63 (13)C6—C7—C8—C9179.50 (18)
F4—P1—F1—Cu1−107.43 (14)N3—C8—C9—N42.0 (3)
F5—P1—F1—Cu172.73 (14)N3—C8—C9—C10−178.19 (14)
Cu1i—N1—C1—C2−174.59 (12)C7—C8—C9—N4−177.58 (19)
Cu1i—N1—C5—C4175.38 (11)C7—C8—C9—C102.3 (4)
Cu1i—N1—C5—C6−4.49 (18)N4—C9—C10—C110.2 (3)
C1—N1—C5—C40.1 (3)C8—C9—C10—C11−179.59 (15)
C1—N1—C5—C6−179.75 (15)C9—C10—C11—C120.1 (3)
C5—N1—C1—C2−0.3 (3)C10—C11—C12—C13−0.4 (3)
Cu1i—N2—N3—Cu1−3.0 (3)C11—C12—C13—N40.4 (4)
D—H···AD—HH···AD···AD—H···A
C3—H3···F3ii0.952.313.257 (3)175
C11—H7···F2iii0.952.543.451 (3)162
C12—H8···F5iv0.952.603.456 (3)150
C13—H9···F3iv0.952.523.226 (3)131
Table 1

Selected bond lengths (Å)

Cu1—F12.4027 (14)
Cu1—N1i 2.0698 (15)
Cu1—N2i 1.9393 (16)
Cu1—N31.9405 (15)
Cu1—N42.0577 (17)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
C3—H3⋯F3ii 0.952.313.257 (3)175
C11—H7⋯F2iii 0.952.543.451 (3)162
C12—H8⋯F5iv 0.952.603.456 (3)150
C13—H9⋯F3iv 0.952.523.226 (3)131

Symmetry codes: (ii) ; (iii) ; (iv) .

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