Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100020503/jz1434sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100020503/jz1434Isup2.hkl |
CCDC reference: 163883
Data collection: EXPOSE in IPDS (Stoe & Cie, 1999); cell refinement: CELL in IPDS; data reduction: INTEGRATE in IPDS; program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXL97.
[Cu(C10H8N2)2(C2N3)]BF4 | F(000) = 2136 |
Mr = 528.77 | Dx = 1.582 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 8000 reflections |
a = 8.6469 (5) Å | θ = 10.6–29.5° |
b = 17.8651 (8) Å | µ = 1.04 mm−1 |
c = 28.7434 (15) Å | T = 193 K |
V = 4440.2 (4) Å3 | Prism, blue |
Z = 8 | 0.35 × 0.24 × 0.11 mm |
Stoe IPDS diffractometer | 2958 reflections with I > 2σ(I) |
Radiation source: sealed tube | Rint = 0.065 |
Graphite monochromator | θmax = 27.5°, θmin = 2.7° |
φ–scan | h = −11→11 |
28872 measured reflections | k = −23→17 |
5090 independent reflections | l = −37→37 |
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)] = 0.045 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.141 | H-atom parameters constrained |
S = 0.87 | w = 1/[σ2(Fo2) + (0.0938P)2] where P = (Fo2 + 2Fc2)/3 |
5090 reflections | (Δ/σ)max < 0.001 |
316 parameters | Δρmax = 0.55 e Å−3 |
0 restraints | Δρmin = −0.56 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Cu | 0.02347 (5) | 0.05718 (2) | 0.128154 (13) | 0.03353 (13) | |
N1 | 0.0343 (3) | 0.10195 (16) | 0.06423 (9) | 0.0352 (6) | |
N2 | 0.1809 (3) | −0.01825 (16) | 0.09480 (9) | 0.0338 (6) | |
N3 | 0.0207 (3) | 0.01521 (17) | 0.19260 (9) | 0.0361 (6) | |
N4 | 0.1559 (3) | 0.13565 (17) | 0.16110 (10) | 0.0349 (6) | |
C5 | −0.3168 (4) | 0.0442 (2) | 0.11144 (11) | 0.0366 (8) | |
N5 | −0.1942 (4) | 0.02240 (19) | 0.11544 (10) | 0.0421 (7) | |
C6 | −0.5069 (4) | 0.1143 (2) | 0.07984 (13) | 0.0439 (8) | |
N6 | −0.5591 (4) | 0.1578 (2) | 0.05507 (13) | 0.0575 (9) | |
N7 | −0.4608 (4) | 0.0630 (2) | 0.10994 (13) | 0.0531 (9) | |
C11 | 0.1244 (4) | 0.0669 (2) | 0.03276 (10) | 0.0347 (7) | |
C12 | −0.0469 (5) | 0.1621 (2) | 0.05169 (12) | 0.0433 (8) | |
H12 | −0.1117 | 0.1843 | 0.0735 | 0.052* | |
C13 | −0.0391 (5) | 0.1927 (2) | 0.00781 (13) | 0.0481 (9) | |
H13 | −0.0946 | 0.2356 | 0.0002 | 0.058* | |
C14 | 0.0542 (5) | 0.1575 (3) | −0.02473 (13) | 0.0508 (10) | |
H14 | 0.0623 | 0.1767 | −0.0547 | 0.061* | |
C15 | 0.1352 (5) | 0.0939 (2) | −0.01233 (12) | 0.0447 (9) | |
H15 | 0.1965 | 0.0694 | −0.0341 | 0.054* | |
C21 | 0.2093 (4) | 0.0005 (2) | 0.04995 (11) | 0.0358 (7) | |
C22 | 0.2564 (4) | −0.0757 (2) | 0.11335 (13) | 0.0421 (8) | |
H22 | 0.2371 | −0.0880 | 0.1443 | 0.050* | |
C23 | 0.3625 (5) | −0.1180 (2) | 0.08877 (16) | 0.0526 (10) | |
H23 | 0.4138 | −0.1578 | 0.1028 | 0.063* | |
C24 | 0.3901 (5) | −0.0996 (3) | 0.04285 (17) | 0.0571 (11) | |
H24 | 0.4601 | −0.1273 | 0.0253 | 0.068* | |
C25 | 0.3133 (5) | −0.0401 (2) | 0.02323 (15) | 0.0480 (9) | |
H25 | 0.3309 | −0.0272 | −0.0077 | 0.058* | |
C31 | 0.0921 (4) | 0.0568 (2) | 0.22517 (11) | 0.0368 (7) | |
C32 | −0.0493 (4) | −0.0489 (2) | 0.20453 (12) | 0.0419 (8) | |
H32 | −0.0994 | −0.0769 | 0.1818 | 0.050* | |
C33 | −0.0486 (5) | −0.0742 (2) | 0.24997 (13) | 0.0479 (9) | |
H33 | −0.0938 | −0.1199 | 0.2576 | 0.057* | |
C34 | 0.0201 (5) | −0.0310 (3) | 0.28382 (13) | 0.0526 (10) | |
H34 | 0.0186 | −0.0462 | 0.3148 | 0.063* | |
C35 | 0.0911 (5) | 0.0351 (3) | 0.27136 (13) | 0.0494 (10) | |
H35 | 0.1380 | 0.0649 | 0.2938 | 0.059* | |
C41 | 0.1739 (4) | 0.1238 (2) | 0.20742 (12) | 0.0378 (8) | |
C42 | 0.2317 (4) | 0.1927 (2) | 0.14149 (13) | 0.0416 (8) | |
H42 | 0.2181 | 0.2018 | 0.1099 | 0.050* | |
C43 | 0.3296 (5) | 0.2386 (2) | 0.16660 (15) | 0.0522 (10) | |
H43 | 0.3849 | 0.2763 | 0.1518 | 0.063* | |
C44 | 0.3443 (5) | 0.2279 (3) | 0.21347 (16) | 0.0577 (11) | |
H44 | 0.4074 | 0.2592 | 0.2310 | 0.069* | |
C45 | 0.2635 (5) | 0.1696 (2) | 0.23467 (14) | 0.0501 (9) | |
H45 | 0.2702 | 0.1618 | 0.2666 | 0.060* | |
B | 0.7986 (6) | 0.2735 (3) | 0.15657 (16) | 0.0473 (10) | |
F1 | 0.7910 (4) | 0.30323 (19) | 0.11285 (11) | 0.0902 (10) | |
F2 | 0.6847 (4) | 0.29696 (19) | 0.18618 (14) | 0.0942 (11) | |
F3 | 0.9396 (4) | 0.2935 (2) | 0.17580 (11) | 0.0827 (9) | |
F4 | 0.7954 (4) | 0.19601 (15) | 0.15373 (9) | 0.0703 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu | 0.0399 (2) | 0.0366 (2) | 0.02407 (19) | 0.00073 (18) | −0.00001 (16) | 0.00167 (16) |
N1 | 0.0436 (15) | 0.0364 (15) | 0.0256 (12) | −0.0007 (13) | 0.0005 (11) | 0.0024 (11) |
N2 | 0.0335 (14) | 0.0359 (15) | 0.0321 (13) | 0.0016 (12) | 0.0014 (11) | −0.0021 (12) |
N3 | 0.0421 (15) | 0.0405 (16) | 0.0258 (12) | 0.0013 (13) | −0.0031 (11) | 0.0019 (11) |
N4 | 0.0349 (15) | 0.0377 (16) | 0.0321 (14) | 0.0010 (12) | 0.0001 (11) | −0.0031 (12) |
C5 | 0.0392 (19) | 0.044 (2) | 0.0268 (14) | −0.0083 (16) | 0.0009 (13) | 0.0047 (14) |
N5 | 0.0431 (18) | 0.0502 (19) | 0.0330 (14) | 0.0000 (14) | −0.0003 (12) | 0.0071 (13) |
C6 | 0.039 (2) | 0.052 (2) | 0.0403 (18) | 0.0016 (17) | 0.0018 (15) | 0.0066 (17) |
N6 | 0.054 (2) | 0.066 (2) | 0.0521 (19) | 0.0072 (18) | 0.0022 (16) | 0.0158 (18) |
N7 | 0.0383 (17) | 0.066 (2) | 0.0547 (19) | −0.0005 (16) | 0.0041 (14) | 0.0205 (17) |
C11 | 0.0393 (17) | 0.0409 (19) | 0.0237 (14) | −0.0072 (15) | 0.0027 (12) | −0.0017 (14) |
C12 | 0.056 (2) | 0.0393 (19) | 0.0350 (17) | 0.0078 (17) | −0.0019 (16) | 0.0086 (15) |
C13 | 0.056 (2) | 0.045 (2) | 0.043 (2) | −0.0017 (19) | −0.0060 (18) | 0.0082 (17) |
C14 | 0.058 (2) | 0.060 (3) | 0.0349 (18) | −0.013 (2) | −0.0030 (16) | 0.0122 (18) |
C15 | 0.047 (2) | 0.055 (2) | 0.0314 (17) | −0.0092 (18) | 0.0033 (15) | −0.0007 (17) |
C21 | 0.0352 (17) | 0.0407 (19) | 0.0314 (16) | −0.0035 (15) | 0.0062 (13) | −0.0058 (14) |
C22 | 0.0424 (19) | 0.040 (2) | 0.0444 (18) | 0.0058 (15) | −0.0004 (16) | 0.0037 (15) |
C23 | 0.051 (2) | 0.042 (2) | 0.065 (3) | 0.0081 (18) | 0.001 (2) | 0.001 (2) |
C24 | 0.050 (2) | 0.051 (2) | 0.070 (3) | 0.009 (2) | 0.017 (2) | −0.008 (2) |
C25 | 0.046 (2) | 0.050 (2) | 0.048 (2) | 0.0007 (18) | 0.0117 (17) | −0.0048 (17) |
C31 | 0.0413 (18) | 0.0438 (19) | 0.0254 (15) | 0.0050 (17) | −0.0005 (13) | −0.0023 (15) |
C32 | 0.053 (2) | 0.041 (2) | 0.0322 (17) | −0.0057 (17) | 0.0006 (15) | 0.0060 (15) |
C33 | 0.056 (3) | 0.050 (2) | 0.0366 (18) | −0.0031 (19) | 0.0013 (17) | 0.0100 (16) |
C34 | 0.067 (3) | 0.065 (3) | 0.0265 (16) | 0.000 (2) | 0.0015 (17) | 0.0108 (17) |
C35 | 0.059 (2) | 0.059 (3) | 0.0302 (17) | 0.000 (2) | −0.0036 (16) | −0.0021 (16) |
C41 | 0.0407 (19) | 0.0398 (19) | 0.0329 (16) | 0.0058 (16) | −0.0051 (14) | −0.0069 (14) |
C42 | 0.044 (2) | 0.0363 (19) | 0.0441 (18) | −0.0036 (16) | 0.0021 (15) | 0.0021 (16) |
C43 | 0.053 (2) | 0.044 (2) | 0.059 (2) | −0.0025 (19) | −0.001 (2) | 0.005 (2) |
C44 | 0.058 (3) | 0.053 (3) | 0.062 (3) | −0.010 (2) | −0.012 (2) | −0.010 (2) |
C45 | 0.059 (2) | 0.049 (2) | 0.0424 (19) | −0.002 (2) | −0.0067 (18) | −0.0044 (17) |
B | 0.047 (2) | 0.047 (3) | 0.047 (2) | −0.002 (2) | 0.0055 (19) | −0.004 (2) |
F1 | 0.117 (3) | 0.083 (2) | 0.0704 (18) | −0.014 (2) | −0.0296 (18) | 0.0259 (17) |
F2 | 0.083 (2) | 0.071 (2) | 0.128 (3) | 0.0178 (17) | 0.051 (2) | −0.0062 (19) |
F3 | 0.0730 (19) | 0.096 (2) | 0.0791 (19) | −0.0129 (17) | −0.0115 (16) | −0.0048 (17) |
F4 | 0.105 (2) | 0.0483 (15) | 0.0575 (15) | −0.0069 (15) | 0.0180 (14) | −0.0088 (11) |
Cu—N3 | 1.998 (3) | C13—C14 | 1.386 (6) |
Cu—N1 | 2.006 (3) | C14—C15 | 1.381 (6) |
Cu—N5 | 2.015 (3) | C21—C25 | 1.387 (5) |
Cu—N4 | 2.043 (3) | C22—C23 | 1.383 (6) |
Cu—N2 | 2.142 (3) | C23—C24 | 1.381 (6) |
N1—C12 | 1.334 (5) | C24—C25 | 1.374 (6) |
N1—C11 | 1.348 (4) | C31—C35 | 1.383 (5) |
N2—C22 | 1.328 (5) | C31—C41 | 1.481 (5) |
N2—C21 | 1.355 (4) | C32—C33 | 1.383 (5) |
N3—C32 | 1.339 (5) | C33—C34 | 1.377 (6) |
N3—C31 | 1.345 (4) | C34—C35 | 1.379 (6) |
N4—C42 | 1.337 (5) | C41—C45 | 1.372 (5) |
N4—C41 | 1.357 (4) | C42—C43 | 1.381 (6) |
C5—N5 | 1.135 (5) | C43—C44 | 1.367 (6) |
C5—N7 | 1.291 (5) | C44—C45 | 1.395 (6) |
C6—N6 | 1.146 (5) | B—F2 | 1.367 (5) |
C6—N7 | 1.322 (5) | B—F1 | 1.366 (6) |
C11—C15 | 1.386 (5) | B—F3 | 1.385 (6) |
C11—C21 | 1.480 (5) | B—F4 | 1.388 (6) |
C12—C13 | 1.376 (5) | ||
N3—Cu—N1 | 177.52 (12) | C12—C13—C14 | 117.9 (4) |
N3—Cu—N5 | 92.35 (12) | C15—C14—C13 | 119.6 (3) |
N1—Cu—N5 | 90.03 (12) | C14—C15—C11 | 119.6 (4) |
N3—Cu—N4 | 80.48 (12) | N2—C21—C25 | 121.0 (3) |
N1—Cu—N4 | 97.17 (12) | N2—C21—C11 | 115.2 (3) |
N5—Cu—N4 | 145.00 (13) | C25—C21—C11 | 123.8 (3) |
N3—Cu—N2 | 100.75 (12) | N2—C22—C23 | 122.9 (4) |
N1—Cu—N2 | 79.11 (11) | C22—C23—C24 | 118.2 (4) |
N5—Cu—N2 | 108.55 (12) | C25—C24—C23 | 119.6 (4) |
N4—Cu—N2 | 106.44 (11) | C24—C25—C21 | 119.4 (4) |
C12—N1—C11 | 119.8 (3) | N3—C31—C35 | 120.7 (4) |
C12—N1—Cu | 123.0 (2) | N3—C31—C41 | 115.2 (3) |
C11—N1—Cu | 117.2 (2) | C35—C31—C41 | 124.0 (3) |
C22—N2—C21 | 118.9 (3) | N3—C32—C33 | 121.3 (3) |
C22—N2—Cu | 128.2 (2) | C34—C33—C32 | 119.1 (4) |
C21—N2—Cu | 112.7 (2) | C33—C34—C35 | 119.3 (3) |
C32—N3—C31 | 120.1 (3) | C34—C35—C31 | 119.5 (4) |
C32—N3—Cu | 124.3 (2) | N4—C41—C45 | 122.1 (4) |
C31—N3—Cu | 115.6 (2) | N4—C41—C31 | 114.2 (3) |
C42—N4—C41 | 118.5 (3) | C45—C41—C31 | 123.7 (3) |
C42—N4—Cu | 127.1 (2) | N4—C42—C43 | 122.2 (4) |
C41—N4—Cu | 114.3 (2) | C44—C43—C42 | 119.3 (4) |
N5—C5—N7 | 173.7 (4) | C43—C44—C45 | 119.2 (4) |
C5—N5—Cu | 141.7 (3) | C41—C45—C44 | 118.6 (4) |
N6—C6—N7 | 174.3 (4) | F2—B—F1 | 114.8 (4) |
C5—N7—C6 | 119.6 (3) | F2—B—F3 | 107.9 (4) |
N1—C11—C15 | 120.3 (3) | F1—B—F3 | 108.0 (4) |
N1—C11—C21 | 115.8 (3) | F2—B—F4 | 109.1 (4) |
C15—C11—C21 | 123.9 (3) | F1—B—F4 | 109.4 (4) |
N1—C12—C13 | 122.8 (4) | F3—B—F4 | 107.4 (4) |
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