(Acetonitrile){hydridotris[3,5-bis­(trifluoro­meth­yl)-1-pyrazol­yl]borato}copper(I)

The title compound, [Cu(C₁₅H₄BF₁₈N₆)(C₂H₃N)] or [HB(3,5-(CF₃)₂Pz)₃]Cu^I(CH₃CN), was synthesized from [Cu^I(CF₃SO₃)]₂·C₆H₅CH₃ and [HB(3,5-(CF₃)₂Pz)₃]Na(H₂O) in CH₂Cl₂/CH₃CN. The Cu^I atom adopts a distorted tetra­hedral geometry and is coordinated by four N atoms, three N atoms from the tridentate tris­(pyrazol­yl)borate ligand [Cu-N = 2.0992 (12) Å] and one N atom from acetonitrile [Cu-N = 1.888 (3) Å]. The acetonitrile ligand is linear. The Cu atom, acetonitrile ligand, B and its attached H atom lie on a crystallographic threefold rotation axis.

checkCIF/PLATON results

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Datablock: I


Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.07
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.47 Ratio
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Cu1    -   N1      ..       7.79 su
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C3
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.11

Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
            correct. If it is not, please give the correct count in the
            _publ_section_exptl_refinement section of the submitted CIF.
           From the CIF: _diffrn_reflns_theta_max           32.62
           From the CIF: _reflns_number_total               2907
           Count of symmetry unique reflns         1505
           Completeness (_total/calc)            193.16%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1402
           Fraction of Friedel pairs measured     0.932
           Are heavy atom types Z>Si present        yes

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

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

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: ORTEP-3 for Windows (Faruggia, 1997).

(Acetonitrile){hydridotris[3,5-bis(trifluoromethyl)-1- pyrazolyl]borato}copper(I)

Crystal data

[Cu(C15H4BF18N6)(C2H3N)]	Dx = 1.957 Mg m^−3
Mr = 725.65	Mo Kα radiation, λ = 0.71073 Å
Trigonal, R3c	Cell parameters from 7594 reflections
Hall symbol: R 3 -2"c	θ = 2.4–32.0°
a = 13.0510 (14) Å	µ = 1.05 mm^−1
c = 25.047 (5) Å	T = 150 K
V = 3694.7 (9) Å^3	Prisms, colorless
Z = 6	0.40 × 0.37 × 0.30 mm
F(000) = 2123.8

Data collection

Bruker SMART APEXII diffractometer	2907 independent reflections
Radiation source: fine-focus sealed tube	2601 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
φ and ω scans	θmax = 32.6°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −19→19
Tmin = 0.664, Tmax = 0.735	k = −19→19
14977 measured reflections	l = −37→37

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.027	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.072	w = 1/[σ^2(Fo^2) + (0.0473P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = 0.001
2907 reflections	Δρmax = 0.48 e Å^−3
136 parameters	Δρmin = −0.23 e Å^−3
1 restraint	Absolute structure: Flack (1983)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.007 (10)

Special details

Experimental. ¹H NMR (300 MHz, C₆D₆, 298 K): δ 6.24 (s, 3H), 0.70 (s, 3H, CH₃CN).

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	Occ. (<1)
Cu1	0.6667	0.3333	0.893096 (15)	0.02801 (8)
C1	0.6667	0.3333	0.77220 (15)	0.0316 (7)
N2	0.77043 (10)	0.28976 (11)	0.94166 (4)	0.0234 (2)
F4	0.87543 (12)	0.37598 (11)	1.10185 (5)	0.0506 (3)
C6	0.82907 (12)	0.26897 (13)	1.02169 (5)	0.0260 (2)
N3	0.75603 (10)	0.29702 (10)	0.99484 (4)	0.02097 (19)
C5	0.89239 (14)	0.24298 (15)	0.98566 (6)	0.0324 (3)
H5	0.9488	0.2211	0.9926	0.039*
F5	0.73799 (12)	0.19505 (13)	1.10518 (5)	0.0484 (3)
C7	0.83937 (15)	0.26972 (16)	1.08104 (6)	0.0338 (3)
F6	0.91834 (13)	0.23762 (14)	1.09492 (4)	0.0508 (3)
F3	1.00119 (10)	0.26550 (16)	0.88275 (5)	0.0650 (4)
C4	0.85182 (12)	0.25732 (13)	0.93638 (6)	0.0276 (3)
F2	0.82784 (13)	0.12369 (13)	0.86898 (6)	0.0626 (4)
N1	0.6667	0.3333	0.81771 (10)	0.0336 (5)
C3	0.88876 (14)	0.23692 (16)	0.88271 (6)	0.0350 (3)
C2	0.6667	0.3333	0.71351 (12)	0.0396 (7)
H2A	0.5883	0.2798	0.7007	0.059*	0.33
H2B	0.7202	0.3085	0.7007	0.059*	0.33
H2C	0.6915	0.4117	0.7007	0.059*	0.33
F1	0.8724 (2)	0.2952 (2)	0.84425 (6)	0.0871 (6)
B1	0.6667	0.3333	1.01603 (12)	0.0189 (5)
H1	0.6667	0.3333	1.0580 (15)	0.017 (8)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cu1	0.03419 (10)	0.03419 (10)	0.01567 (11)	0.01709 (5)	0.000	0.000
C1	0.0348 (10)	0.0348 (10)	0.0252 (15)	0.0174 (5)	0.000	0.000
N2	0.0253 (5)	0.0268 (5)	0.0187 (4)	0.0135 (4)	0.0007 (4)	−0.0030 (4)
F4	0.0720 (8)	0.0580 (7)	0.0344 (5)	0.0419 (6)	−0.0256 (5)	−0.0215 (5)
C6	0.0269 (6)	0.0324 (7)	0.0235 (6)	0.0184 (6)	−0.0050 (5)	−0.0056 (5)
N3	0.0224 (5)	0.0244 (5)	0.0175 (4)	0.0128 (4)	−0.0017 (4)	−0.0023 (4)
C5	0.0312 (7)	0.0467 (8)	0.0290 (7)	0.0267 (6)	−0.0056 (5)	−0.0093 (6)
F5	0.0538 (6)	0.0719 (7)	0.0293 (5)	0.0389 (6)	0.0057 (4)	0.0126 (5)
C7	0.0399 (8)	0.0482 (9)	0.0253 (6)	0.0311 (8)	−0.0093 (5)	−0.0064 (6)
F6	0.0603 (7)	0.0860 (9)	0.0351 (5)	0.0583 (7)	−0.0125 (4)	−0.0035 (5)
F3	0.0334 (5)	0.0985 (10)	0.0565 (8)	0.0280 (6)	0.0040 (5)	−0.0343 (7)
C4	0.0277 (6)	0.0333 (7)	0.0244 (6)	0.0172 (5)	0.0002 (5)	−0.0057 (5)
F2	0.0554 (7)	0.0619 (8)	0.0516 (7)	0.0151 (6)	0.0102 (6)	−0.0296 (7)
N1	0.0395 (7)	0.0395 (7)	0.0219 (10)	0.0197 (4)	0.000	0.000
C3	0.0340 (7)	0.0459 (9)	0.0302 (7)	0.0239 (7)	0.0031 (5)	−0.0075 (6)
C2	0.0508 (11)	0.0508 (11)	0.0174 (12)	0.0254 (5)	0.000	0.000
F1	0.1534 (16)	0.1412 (16)	0.0346 (6)	0.1245 (15)	0.0339 (8)	0.0241 (8)
B1	0.0212 (8)	0.0212 (8)	0.0145 (12)	0.0106 (4)	0.000	0.000

Geometric parameters (Å, º)

Cu1—N1	1.888 (3)	C5—H5	0.9300
Cu1—N2^i	2.0992 (12)	F5—C7	1.333 (2)
Cu1—N2^ii	2.0992 (12)	C7—F6	1.3381 (18)
Cu1—N2	2.0992 (12)	F3—C3	1.321 (2)
C1—N1	1.140 (5)	C4—C3	1.496 (2)
C1—C2	1.470 (5)	F2—C3	1.326 (2)
N2—C4	1.3322 (18)	C3—F1	1.309 (2)
N2—N3	1.3553 (15)	C2—H2A	0.9600
F4—C7	1.328 (2)	C2—H2B	0.9600
C6—N3	1.3578 (17)	C2—H2C	0.9600
C6—C5	1.3758 (18)	B1—N3^ii	1.5554 (15)
C6—C7	1.492 (2)	B1—N3^i	1.5554 (15)
N3—B1	1.5554 (15)	B1—H1	1.05 (4)
C5—C4	1.392 (2)
N1—Cu1—N2^i	125.41 (3)	F6—C7—C6	109.74 (12)
N1—Cu1—N2^ii	125.41 (3)	N2—C4—C5	111.85 (12)
N2^i—Cu1—N2^ii	89.80 (5)	N2—C4—C3	121.64 (13)
N1—Cu1—N2	125.41 (3)	C5—C4—C3	126.49 (13)
N2^i—Cu1—N2	89.79 (5)	C1—N1—Cu1	180.000 (1)
N2^ii—Cu1—N2	89.79 (5)	F1—C3—F3	108.51 (17)
N1—C1—C2	180.000 (2)	F1—C3—F2	105.98 (17)
C4—N2—N3	106.26 (11)	F3—C3—F2	106.09 (15)
C4—N2—Cu1	138.90 (10)	F1—C3—C4	113.40 (14)
N3—N2—Cu1	114.82 (8)	F3—C3—C4	111.12 (13)
N3—C6—C5	109.32 (12)	F2—C3—C4	111.36 (14)
N3—C6—C7	124.38 (12)	C1—C2—H2A	109.5
C5—C6—C7	126.29 (12)	C1—C2—H2B	109.5
N2—N3—C6	109.11 (10)	H2A—C2—H2B	109.5
N2—N3—B1	120.52 (14)	C1—C2—H2C	109.5
C6—N3—B1	130.37 (14)	H2A—C2—H2C	109.5
C6—C5—C4	103.46 (12)	H2B—C2—H2C	109.5
C6—C5—H5	128.3	N3—B1—N3^ii	108.99 (12)
C4—C5—H5	128.3	N3—B1—N3^i	108.99 (12)
F4—C7—F5	106.83 (14)	N3^ii—B1—N3^i	108.99 (12)
F4—C7—F6	107.38 (13)	N3—B1—H1	109.94 (11)
F5—C7—F6	106.96 (14)	N3^ii—B1—H1	109.95 (12)
F4—C7—C6	112.43 (14)	N3^i—B1—H1	109.95 (12)
F5—C7—C6	113.19 (13)

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