The molecule of the title compound, [Cu
2(N
3)
2(C
9H
10BN
6)
2], is located at a crystallographic inversion centre. The two Cu atoms have distorted square-pyramidal coordination and are bridged by two end-on azide groups. Weak C—H
N contacts result in a two-dimensional network with base vectors [101] and [010], parallel to the (10
) plane.
Supporting information
CCDC reference: 238635
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å
- R factor = 0.049
- wR factor = 0.110
- Data-to-parameter ratio = 14.4
checkCIF/PLATON results
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Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Bis(µ
2-azido)-bis(hydrotris(1-pyrazolyl)borato)-di-copper(II)
top
Crystal data top
[Cu2(N3)2(C9H10BN6)2] | F(000) = 644 |
Mr = 637.22 | Dx = 1.590 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 1028 reflections |
a = 7.515 (1) Å | θ = 2.2–19.8° |
b = 13.363 (2) Å | µ = 1.64 mm−1 |
c = 13.285 (2) Å | T = 293 K |
β = 93.65 (1)° | Block, green |
V = 1331.4 (3) Å3 | 0.3 × 0.2 × 0.2 mm |
Z = 2 | |
Data collection top
Bruker SMART Apex CCD area-detector diffractometer | 2605 independent reflections |
Radiation source: sealed tube | 2000 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 26.0°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −4→9 |
Tmin = 0.68, Tmax = 0.72 | k = −15→16 |
6976 measured reflections | l = −16→15 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.110 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.05P)2 + 1.22P] where P = (Fo2 + 2Fc2)/3 |
2605 reflections | (Δ/σ)max < 0.001 |
181 parameters | Δρmax = 0.61 e Å−3 |
0 restraints | Δρmin = −0.76 e Å−3 |
Special details top
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 | x | y | z | Uiso*/Ueq | |
Cu1 | 0.85233 (7) | 0.98092 (3) | 0.41336 (3) | 0.04239 (18) | |
B1 | 0.6835 (6) | 0.9369 (3) | 0.2014 (3) | 0.0419 (10) | |
H10A | 0.6218 | 0.9237 | 0.1355 | 0.050* | |
N1 | 0.8849 (4) | 0.9397 (2) | 0.1916 (2) | 0.0362 (7) | |
N2 | 0.9955 (4) | 0.9610 (2) | 0.2727 (2) | 0.0382 (7) | |
N3 | 0.6214 (4) | 1.0368 (2) | 0.2432 (2) | 0.0396 (7) | |
N4 | 0.6708 (5) | 1.0646 (2) | 0.3388 (2) | 0.0488 (8) | |
N5 | 0.6419 (4) | 0.8534 (2) | 0.2766 (2) | 0.0386 (7) | |
N6 | 0.7071 (4) | 0.8589 (2) | 0.3742 (2) | 0.0420 (8) | |
C1 | 0.9791 (6) | 0.9235 (3) | 0.1112 (3) | 0.0466 (10) | |
H1 | 0.9319 | 0.9088 | 0.0465 | 0.056* | |
C2 | 1.1572 (6) | 0.9321 (3) | 0.1399 (3) | 0.0545 (11) | |
H2 | 1.2541 | 0.9238 | 0.1005 | 0.065* | |
C3 | 1.1579 (5) | 0.9559 (3) | 0.2410 (3) | 0.0454 (10) | |
H3 | 1.2610 | 0.9669 | 0.2821 | 0.054* | |
C4 | 0.5131 (5) | 1.1052 (3) | 0.2011 (3) | 0.0515 (11) | |
H4 | 0.4596 | 1.1020 | 0.1361 | 0.062* | |
C5 | 0.4926 (6) | 1.1806 (3) | 0.2678 (4) | 0.0601 (12) | |
H5 | 0.4268 | 1.2391 | 0.2576 | 0.072* | |
C6 | 0.5896 (6) | 1.1516 (3) | 0.3530 (3) | 0.0565 (11) | |
H6 | 0.5980 | 1.1878 | 0.4129 | 0.068* | |
C7 | 0.5496 (6) | 0.7683 (3) | 0.2647 (3) | 0.0501 (10) | |
H7 | 0.4899 | 0.7473 | 0.2050 | 0.060* | |
C8 | 0.5562 (6) | 0.7168 (3) | 0.3541 (3) | 0.0593 (12) | |
H8 | 0.5047 | 0.6553 | 0.3672 | 0.071* | |
C9 | 0.6558 (6) | 0.7765 (3) | 0.4193 (3) | 0.0541 (11) | |
H9 | 0.6839 | 0.7612 | 0.4868 | 0.065* | |
N7 | 1.0209 (4) | 0.9074 (2) | 0.5096 (2) | 0.0435 (8) | |
N8 | 1.0691 (5) | 0.8246 (2) | 0.4967 (2) | 0.0438 (8) | |
N9 | 1.1128 (5) | 0.7433 (3) | 0.4845 (2) | 0.0548 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0557 (3) | 0.0328 (3) | 0.0380 (3) | 0.0017 (2) | −0.0018 (2) | −0.0037 (2) |
B1 | 0.050 (3) | 0.038 (2) | 0.037 (2) | −0.005 (2) | −0.001 (2) | 0.0006 (18) |
N1 | 0.0418 (18) | 0.0318 (16) | 0.0350 (16) | −0.0020 (13) | 0.0032 (14) | −0.0021 (12) |
N2 | 0.0415 (18) | 0.0382 (18) | 0.0345 (16) | −0.0032 (14) | −0.0005 (13) | −0.0005 (12) |
N3 | 0.0369 (17) | 0.0325 (17) | 0.0487 (19) | −0.0007 (14) | −0.0018 (14) | 0.0023 (13) |
N4 | 0.061 (2) | 0.0352 (18) | 0.050 (2) | 0.0059 (17) | 0.0028 (17) | −0.0071 (15) |
N5 | 0.0389 (18) | 0.0346 (17) | 0.0433 (18) | −0.0011 (14) | 0.0099 (14) | −0.0020 (13) |
N6 | 0.0465 (19) | 0.0402 (18) | 0.0399 (17) | −0.0074 (15) | 0.0083 (15) | 0.0031 (14) |
C1 | 0.067 (3) | 0.040 (2) | 0.034 (2) | −0.006 (2) | 0.0079 (19) | −0.0024 (16) |
C2 | 0.053 (3) | 0.052 (3) | 0.061 (3) | 0.002 (2) | 0.022 (2) | −0.003 (2) |
C3 | 0.036 (2) | 0.031 (2) | 0.069 (3) | −0.0031 (16) | 0.007 (2) | 0.0034 (18) |
C4 | 0.042 (2) | 0.041 (2) | 0.071 (3) | −0.0018 (19) | −0.003 (2) | 0.013 (2) |
C5 | 0.052 (3) | 0.041 (2) | 0.086 (3) | 0.016 (2) | 0.001 (2) | 0.003 (2) |
C6 | 0.059 (3) | 0.044 (3) | 0.067 (3) | 0.003 (2) | 0.010 (2) | −0.009 (2) |
C7 | 0.049 (3) | 0.050 (3) | 0.052 (2) | −0.004 (2) | 0.010 (2) | −0.0072 (19) |
C8 | 0.059 (3) | 0.043 (3) | 0.077 (3) | −0.015 (2) | 0.015 (2) | 0.006 (2) |
C9 | 0.065 (3) | 0.047 (2) | 0.053 (2) | −0.003 (2) | 0.020 (2) | 0.010 (2) |
N7 | 0.057 (2) | 0.0335 (19) | 0.0395 (17) | 0.0015 (15) | −0.0008 (15) | −0.0030 (13) |
N8 | 0.058 (2) | 0.034 (2) | 0.0394 (18) | 0.0016 (17) | −0.0012 (15) | −0.0030 (14) |
N9 | 0.073 (3) | 0.043 (2) | 0.048 (2) | 0.0011 (19) | 0.0018 (18) | 0.0031 (16) |
Geometric parameters (Å, º) top
Cu1—N4 | 1.980 (3) | C1—C2 | 1.372 (6) |
Cu1—N7 | 2.000 (3) | C1—H1 | 0.9300 |
Cu1—N6 | 2.012 (3) | C2—C3 | 1.381 (6) |
Cu1—N7i | 2.015 (3) | C2—H2 | 0.9300 |
Cu1—N2 | 2.231 (3) | C3—H3 | 0.9300 |
B1—N1 | 1.528 (5) | C4—C5 | 1.357 (6) |
B1—N3 | 1.530 (5) | C4—H4 | 0.9300 |
B1—N5 | 1.543 (5) | C5—C6 | 1.363 (6) |
B1—H10A | 0.9800 | C5—H5 | 0.9300 |
N1—C1 | 1.336 (5) | C6—H6 | 0.9300 |
N1—N2 | 1.348 (4) | C7—C8 | 1.370 (6) |
N2—C3 | 1.318 (5) | C7—H7 | 0.9300 |
N3—C4 | 1.323 (5) | C8—C9 | 1.365 (6) |
N3—N4 | 1.353 (4) | C8—H8 | 0.9300 |
N4—C6 | 1.332 (5) | C9—H9 | 0.9300 |
N5—C7 | 1.336 (5) | N7—N8 | 1.179 (4) |
N5—N6 | 1.359 (4) | N7—Cu1i | 2.015 (3) |
N6—C9 | 1.323 (5) | N8—N9 | 1.150 (4) |
| | | |
N4—Cu1—N7 | 170.27 (13) | N5—N6—Cu1 | 116.6 (2) |
N4—Cu1—N6 | 89.03 (13) | N1—C1—C2 | 108.8 (3) |
N7—Cu1—N6 | 94.49 (13) | N1—C1—H1 | 125.6 |
N4—Cu1—N7i | 97.14 (13) | C2—C1—H1 | 125.6 |
N7—Cu1—N7i | 77.26 (15) | C1—C2—C3 | 103.5 (4) |
N6—Cu1—N7i | 164.35 (12) | C1—C2—H2 | 128.3 |
N4—Cu1—N2 | 90.11 (12) | C3—C2—H2 | 128.3 |
N7—Cu1—N2 | 99.05 (12) | N2—C3—C2 | 112.1 (4) |
N6—Cu1—N2 | 88.26 (11) | N2—C3—H3 | 124.0 |
N7i—Cu1—N2 | 106.02 (12) | C2—C3—H3 | 124.0 |
N1—B1—N3 | 109.6 (3) | N3—C4—C5 | 109.3 (4) |
N1—B1—N5 | 108.4 (3) | N3—C4—H4 | 125.4 |
N3—B1—N5 | 108.5 (3) | C5—C4—H4 | 125.4 |
N1—B1—H10A | 110.1 | C4—C5—C6 | 104.7 (4) |
N3—B1—H10A | 110.1 | C4—C5—H5 | 127.7 |
N5—B1—H10A | 110.1 | C6—C5—H5 | 127.7 |
C1—N1—N2 | 109.9 (3) | N4—C6—C5 | 110.9 (4) |
C1—N1—B1 | 130.0 (3) | N4—C6—H6 | 124.6 |
N2—N1—B1 | 120.1 (3) | C5—C6—H6 | 124.6 |
C3—N2—N1 | 105.7 (3) | N5—C7—C8 | 109.6 (4) |
C3—N2—Cu1 | 141.2 (3) | N5—C7—H7 | 125.2 |
N1—N2—Cu1 | 112.8 (2) | C8—C7—H7 | 125.2 |
C4—N3—N4 | 109.4 (3) | C9—C8—C7 | 104.2 (4) |
C4—N3—B1 | 130.0 (3) | C9—C8—H8 | 127.9 |
N4—N3—B1 | 120.6 (3) | C7—C8—H8 | 127.9 |
C6—N4—N3 | 105.8 (3) | N6—C9—C8 | 111.2 (4) |
C6—N4—Cu1 | 136.8 (3) | N6—C9—H9 | 124.4 |
N3—N4—Cu1 | 117.0 (2) | C8—C9—H9 | 124.4 |
C7—N5—N6 | 108.2 (3) | N8—N7—Cu1 | 123.8 (3) |
C7—N5—B1 | 131.6 (3) | N8—N7—Cu1i | 128.9 (3) |
N6—N5—B1 | 120.2 (3) | Cu1—N7—Cu1i | 102.74 (15) |
C9—N6—N5 | 106.8 (3) | N9—N8—N7 | 178.7 (4) |
C9—N6—Cu1 | 136.6 (3) | | |
Symmetry code: (i) −x+2, −y+2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4···N9ii | 0.93 | 2.51 | 3.176 (5) | 128 |
Symmetry code: (ii) −x+3/2, y+1/2, −z+1/2. |