Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618009853/qf3015sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229618009853/qf3015Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229618009853/qf3015IIsup3.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618009853/qf3015sup4.pdf |
CCDC references: 1854768; 1854767
For both structures, data collection: IPDS Software (Stoe & Cie, 2000); cell refinement: IPDS Software (Stoe & Cie, 2000); data reduction: IPDS Software (Stoe & Cie, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 2012).
[CuNbF5O(C6H10N2)3] | F(000) = 1212 |
Mr = 597.93 | Dx = 1.616 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.3311 (4) Å | Cell parameters from 8000 reflections |
b = 13.2097 (5) Å | θ = 2.6–27.9° |
c = 19.9741 (9) Å | µ = 1.39 mm−1 |
β = 93.275 (5)° | T = 213 K |
V = 2458.01 (18) Å3 | Prism, blue-green |
Z = 4 | 0.18 × 0.14 × 0.12 mm |
Stoe image plate diffraction system diffractometer | 3683 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.045 |
φ oscillation scans | θmax = 27.9°, θmin = 2.6° |
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)] | h = −11→12 |
Tmin = 0.742, Tmax = 0.789 | k = −17→17 |
20504 measured reflections | l = −26→26 |
5875 independent reflections |
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)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.048 | H-atom parameters constrained |
S = 0.81 | w = 1/[σ2(Fo2) + (0.0156P)2] where P = (Fo2 + 2Fc2)/3 |
5875 reflections | (Δ/σ)max = 0.001 |
298 parameters | Δρmax = 0.42 e Å−3 |
0 restraints | Δρmin = −0.58 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Nb1 | −0.01003 (2) | 0.55369 (2) | 0.28466 (2) | 0.02110 (6) | |
Cu1 | −0.05515 (3) | 0.29853 (2) | 0.35415 (2) | 0.01811 (7) | |
O1 | −0.02317 (16) | 0.44027 (13) | 0.32895 (8) | 0.0287 (4) | |
F1 | 0.01511 (14) | 0.68153 (10) | 0.22280 (7) | 0.0266 (3) | |
F2 | 0.17511 (14) | 0.59753 (11) | 0.32193 (7) | 0.0338 (4) | |
F3 | 0.08481 (15) | 0.49216 (11) | 0.21034 (7) | 0.0360 (4) | |
F4 | −0.18979 (13) | 0.54624 (11) | 0.23210 (7) | 0.0336 (4) | |
F5 | −0.10042 (15) | 0.64102 (12) | 0.34505 (7) | 0.0370 (4) | |
N1 | −0.25274 (19) | 0.31105 (15) | 0.31201 (10) | 0.0214 (4) | |
N2 | −0.2982 (2) | 0.25001 (16) | 0.26095 (10) | 0.0275 (5) | |
H2 | −0.2478 | 0.2010 | 0.2452 | 0.033* | |
N3 | −0.11373 (19) | 0.19313 (15) | 0.42090 (10) | 0.0218 (4) | |
N4 | −0.1383 (2) | 0.09488 (16) | 0.40436 (10) | 0.0262 (5) | |
H4 | −0.1314 | 0.0702 | 0.3643 | 0.031* | |
N5 | 0.15083 (19) | 0.28444 (15) | 0.38533 (9) | 0.0217 (4) | |
N6 | 0.22811 (19) | 0.20595 (16) | 0.36390 (10) | 0.0240 (5) | |
H6 | 0.1977 | 0.1639 | 0.3327 | 0.029* | |
C1 | −0.3614 (2) | 0.37535 (18) | 0.32103 (12) | 0.0234 (5) | |
C2 | −0.4759 (2) | 0.3550 (2) | 0.27476 (13) | 0.0277 (6) | |
C3 | −0.4325 (3) | 0.2750 (2) | 0.23748 (13) | 0.0312 (6) | |
C4 | −0.3505 (3) | 0.4559 (2) | 0.37347 (14) | 0.0366 (6) | |
H4A | −0.2806 | 0.4359 | 0.4088 | 0.055* | |
H4B | −0.4433 | 0.4653 | 0.3921 | 0.055* | |
H4C | −0.3204 | 0.5188 | 0.3536 | 0.055* | |
C5 | −0.6156 (3) | 0.4094 (2) | 0.26729 (15) | 0.0436 (8) | |
H5A | −0.6059 | 0.4680 | 0.2386 | 0.065* | |
H5B | −0.6437 | 0.4313 | 0.3110 | 0.065* | |
H5C | −0.6883 | 0.3645 | 0.2474 | 0.065* | |
C6 | −0.5074 (3) | 0.2175 (3) | 0.18131 (16) | 0.0611 (10) | |
H6A | −0.5848 | 0.1780 | 0.1985 | 0.092* | |
H6B | −0.4397 | 0.1725 | 0.1612 | 0.092* | |
H6C | −0.5463 | 0.2646 | 0.1477 | 0.092* | |
C7 | −0.1364 (2) | 0.1997 (2) | 0.48607 (12) | 0.0248 (5) | |
C8 | −0.1748 (3) | 0.1048 (2) | 0.51116 (13) | 0.0321 (7) | |
C9 | −0.1747 (2) | 0.0404 (2) | 0.45774 (14) | 0.0299 (6) | |
C10 | −0.1186 (3) | 0.2972 (2) | 0.52358 (13) | 0.0389 (7) | |
H10A | −0.0334 | 0.2937 | 0.5537 | 0.058* | |
H10B | −0.2021 | 0.3088 | 0.5494 | 0.058* | |
H10C | −0.1088 | 0.3523 | 0.4921 | 0.058* | |
C11 | −0.2047 (3) | 0.0810 (3) | 0.58272 (14) | 0.0579 (9) | |
H11A | −0.3004 | 0.1040 | 0.5917 | 0.087* | |
H11B | −0.1348 | 0.1152 | 0.6126 | 0.087* | |
H11C | −0.1980 | 0.0085 | 0.5899 | 0.087* | |
C12 | −0.2068 (3) | −0.0710 (2) | 0.45176 (16) | 0.0495 (8) | |
H12A | −0.1537 | −0.1072 | 0.4874 | 0.074* | |
H12B | −0.1785 | −0.0954 | 0.4087 | 0.074* | |
H12C | −0.3088 | −0.0820 | 0.4553 | 0.074* | |
C13 | 0.2344 (3) | 0.33045 (19) | 0.43324 (12) | 0.0259 (6) | |
C14 | 0.3650 (2) | 0.2783 (2) | 0.44213 (12) | 0.0289 (6) | |
C15 | 0.3578 (2) | 0.2004 (2) | 0.39649 (13) | 0.0287 (6) | |
C16 | 0.1900 (3) | 0.4242 (2) | 0.46736 (15) | 0.0448 (8) | |
H16A | 0.0977 | 0.4465 | 0.4479 | 0.067* | |
H16B | 0.2610 | 0.4767 | 0.4617 | 0.067* | |
H16C | 0.1823 | 0.4108 | 0.5148 | 0.067* | |
C17 | 0.4868 (3) | 0.3000 (3) | 0.49242 (15) | 0.0564 (9) | |
H17A | 0.5018 | 0.2422 | 0.5219 | 0.085* | |
H17B | 0.4638 | 0.3590 | 0.5187 | 0.085* | |
H17C | 0.5734 | 0.3129 | 0.4692 | 0.085* | |
C18 | 0.4664 (3) | 0.1224 (2) | 0.37989 (15) | 0.0429 (8) | |
H18A | 0.4265 | 0.0789 | 0.3444 | 0.064* | |
H18B | 0.4915 | 0.0820 | 0.4194 | 0.064* | |
H18C | 0.5517 | 0.1557 | 0.3651 | 0.064* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Nb1 | 0.02041 (10) | 0.01872 (11) | 0.02379 (12) | −0.00274 (10) | −0.00198 (8) | 0.00594 (12) |
Cu1 | 0.01638 (14) | 0.01636 (15) | 0.02126 (15) | 0.00006 (12) | −0.00182 (11) | 0.00246 (14) |
O1 | 0.0257 (8) | 0.0248 (10) | 0.0349 (10) | −0.0038 (8) | −0.0040 (7) | 0.0109 (9) |
F1 | 0.0254 (7) | 0.0227 (7) | 0.0310 (8) | −0.0036 (6) | −0.0032 (6) | 0.0105 (7) |
F2 | 0.0261 (7) | 0.0333 (8) | 0.0407 (9) | −0.0091 (6) | −0.0104 (6) | 0.0100 (7) |
F3 | 0.0412 (9) | 0.0299 (9) | 0.0376 (9) | 0.0087 (7) | 0.0079 (7) | 0.0043 (7) |
F4 | 0.0265 (7) | 0.0347 (9) | 0.0383 (8) | −0.0088 (7) | −0.0102 (6) | 0.0100 (8) |
F5 | 0.0409 (9) | 0.0352 (9) | 0.0352 (9) | 0.0020 (7) | 0.0052 (7) | −0.0024 (8) |
N1 | 0.0190 (10) | 0.0214 (11) | 0.0234 (11) | 0.0024 (8) | −0.0028 (8) | −0.0006 (9) |
N2 | 0.0228 (11) | 0.0275 (12) | 0.0314 (12) | 0.0070 (9) | −0.0043 (9) | −0.0090 (10) |
N3 | 0.0230 (10) | 0.0200 (11) | 0.0221 (11) | 0.0000 (9) | −0.0010 (8) | 0.0038 (10) |
N4 | 0.0266 (11) | 0.0210 (11) | 0.0314 (12) | −0.0008 (9) | 0.0040 (9) | 0.0015 (10) |
N5 | 0.0193 (10) | 0.0209 (11) | 0.0244 (11) | 0.0002 (9) | −0.0027 (8) | −0.0020 (10) |
N6 | 0.0205 (10) | 0.0227 (11) | 0.0284 (11) | 0.0009 (9) | −0.0028 (8) | −0.0034 (10) |
C1 | 0.0221 (12) | 0.0210 (14) | 0.0275 (14) | 0.0040 (10) | 0.0041 (10) | 0.0027 (12) |
C2 | 0.0206 (13) | 0.0313 (15) | 0.0310 (15) | 0.0047 (11) | −0.0001 (11) | 0.0068 (13) |
C3 | 0.0234 (13) | 0.0403 (17) | 0.0289 (15) | 0.0031 (12) | −0.0068 (11) | −0.0008 (13) |
C4 | 0.0322 (14) | 0.0322 (16) | 0.0459 (17) | 0.0068 (13) | 0.0051 (12) | −0.0055 (15) |
C5 | 0.0244 (14) | 0.0499 (19) | 0.056 (2) | 0.0113 (13) | −0.0008 (13) | 0.0049 (16) |
C6 | 0.0423 (18) | 0.079 (3) | 0.059 (2) | 0.0125 (18) | −0.0210 (15) | −0.025 (2) |
C7 | 0.0227 (12) | 0.0289 (14) | 0.0226 (13) | 0.0033 (11) | −0.0011 (10) | 0.0032 (13) |
C8 | 0.0276 (14) | 0.0398 (17) | 0.0294 (15) | 0.0020 (12) | 0.0040 (11) | 0.0162 (14) |
C9 | 0.0244 (13) | 0.0252 (15) | 0.0404 (16) | 0.0004 (11) | 0.0046 (11) | 0.0135 (14) |
C10 | 0.0389 (15) | 0.0475 (18) | 0.0298 (15) | 0.0012 (14) | −0.0008 (12) | −0.0079 (15) |
C11 | 0.068 (2) | 0.071 (3) | 0.0361 (18) | −0.0089 (19) | 0.0100 (16) | 0.0202 (18) |
C12 | 0.0498 (18) | 0.0340 (19) | 0.065 (2) | −0.0083 (14) | 0.0069 (15) | 0.0133 (16) |
C13 | 0.0291 (14) | 0.0266 (15) | 0.0214 (13) | −0.0093 (11) | −0.0021 (11) | 0.0015 (11) |
C14 | 0.0206 (13) | 0.0405 (17) | 0.0247 (14) | −0.0080 (11) | −0.0068 (10) | 0.0075 (13) |
C15 | 0.0193 (12) | 0.0311 (15) | 0.0354 (15) | −0.0014 (11) | −0.0019 (10) | 0.0125 (14) |
C16 | 0.0497 (18) | 0.039 (2) | 0.0448 (18) | −0.0082 (14) | −0.0029 (14) | −0.0157 (15) |
C17 | 0.0402 (17) | 0.079 (2) | 0.0471 (19) | −0.0168 (17) | −0.0203 (14) | 0.0079 (19) |
C18 | 0.0251 (14) | 0.0443 (19) | 0.059 (2) | 0.0084 (13) | 0.0028 (13) | 0.0090 (16) |
Nb1—O1 | 1.7479 (17) | C5—H5B | 0.9700 |
Nb1—F5 | 1.9008 (15) | C5—H5C | 0.9700 |
Nb1—F4 | 1.9298 (12) | C6—H6A | 0.9700 |
Nb1—F2 | 1.9306 (13) | C6—H6B | 0.9700 |
Nb1—F3 | 1.9487 (15) | C6—H6C | 0.9700 |
Nb1—F1 | 2.1134 (13) | C7—C8 | 1.404 (4) |
Cu1—O1 | 1.9660 (17) | C7—C10 | 1.494 (4) |
Cu1—N1 | 1.9895 (18) | C8—C9 | 1.365 (4) |
Cu1—N5 | 1.9950 (18) | C8—C11 | 1.505 (4) |
Cu1—N3 | 2.0244 (19) | C9—C12 | 1.505 (4) |
Cu1—F1i | 2.2262 (13) | C10—H10A | 0.9700 |
F1—Cu1ii | 2.2262 (13) | C10—H10B | 0.9700 |
N1—C1 | 1.342 (3) | C10—H10C | 0.9700 |
N1—N2 | 1.349 (3) | C11—H11A | 0.9700 |
N2—C3 | 1.353 (3) | C11—H11B | 0.9700 |
N2—H2 | 0.8700 | C11—H11C | 0.9700 |
N3—C7 | 1.334 (3) | C12—H12A | 0.9700 |
N3—N4 | 1.356 (3) | C12—H12B | 0.9700 |
N4—C9 | 1.346 (3) | C12—H12C | 0.9700 |
N4—H4 | 0.8700 | C13—C14 | 1.402 (3) |
N5—C13 | 1.345 (3) | C13—C16 | 1.484 (4) |
N5—N6 | 1.347 (3) | C14—C15 | 1.374 (4) |
N6—C15 | 1.343 (3) | C14—C17 | 1.500 (3) |
N6—H6 | 0.8700 | C15—C18 | 1.495 (4) |
C1—C2 | 1.398 (3) | C16—H16A | 0.9700 |
C1—C4 | 1.493 (3) | C16—H16B | 0.9700 |
C2—C3 | 1.367 (4) | C16—H16C | 0.9700 |
C2—C5 | 1.489 (3) | C17—H17A | 0.9700 |
C3—C6 | 1.495 (4) | C17—H17B | 0.9700 |
C4—H4A | 0.9700 | C17—H17C | 0.9700 |
C4—H4B | 0.9700 | C18—H18A | 0.9700 |
C4—H4C | 0.9700 | C18—H18B | 0.9700 |
C5—H5A | 0.9700 | C18—H18C | 0.9700 |
O1—Nb1—F5 | 98.78 (7) | C2—C5—H5C | 109.5 |
O1—Nb1—F4 | 98.49 (7) | H5A—C5—H5C | 109.5 |
F5—Nb1—F4 | 88.44 (6) | H5B—C5—H5C | 109.5 |
O1—Nb1—F2 | 98.57 (6) | C3—C6—H6A | 109.5 |
F5—Nb1—F2 | 89.59 (6) | C3—C6—H6B | 109.5 |
F4—Nb1—F2 | 162.92 (6) | H6A—C6—H6B | 109.5 |
O1—Nb1—F3 | 94.36 (7) | C3—C6—H6C | 109.5 |
F5—Nb1—F3 | 166.85 (6) | H6A—C6—H6C | 109.5 |
F4—Nb1—F3 | 89.01 (6) | H6B—C6—H6C | 109.5 |
F2—Nb1—F3 | 89.06 (6) | N3—C7—C8 | 110.4 (2) |
O1—Nb1—F1 | 173.83 (7) | N3—C7—C10 | 121.8 (2) |
F5—Nb1—F1 | 87.37 (6) | C8—C7—C10 | 127.8 (2) |
F4—Nb1—F1 | 81.07 (5) | C9—C8—C7 | 105.4 (2) |
F2—Nb1—F1 | 81.90 (6) | C9—C8—C11 | 128.3 (3) |
F3—Nb1—F1 | 79.48 (6) | C7—C8—C11 | 126.2 (3) |
O1—Cu1—N1 | 87.89 (7) | N4—C9—C8 | 107.3 (2) |
O1—Cu1—N5 | 90.64 (7) | N4—C9—C12 | 121.2 (3) |
N1—Cu1—N5 | 173.17 (8) | C8—C9—C12 | 131.5 (2) |
O1—Cu1—N3 | 150.96 (8) | C7—C10—H10A | 109.5 |
N1—Cu1—N3 | 93.28 (8) | C7—C10—H10B | 109.5 |
N5—Cu1—N3 | 91.25 (8) | H10A—C10—H10B | 109.5 |
O1—Cu1—F1i | 116.78 (6) | C7—C10—H10C | 109.5 |
N1—Cu1—F1i | 87.34 (7) | H10A—C10—H10C | 109.5 |
N5—Cu1—F1i | 87.37 (7) | H10B—C10—H10C | 109.5 |
N3—Cu1—F1i | 92.26 (7) | C8—C11—H11A | 109.5 |
Nb1—O1—Cu1 | 164.16 (10) | C8—C11—H11B | 109.5 |
Nb1—F1—Cu1ii | 170.74 (7) | H11A—C11—H11B | 109.5 |
C1—N1—N2 | 105.81 (18) | C8—C11—H11C | 109.5 |
C1—N1—Cu1 | 133.19 (17) | H11A—C11—H11C | 109.5 |
N2—N1—Cu1 | 120.92 (14) | H11B—C11—H11C | 109.5 |
N1—N2—C3 | 111.2 (2) | C9—C12—H12A | 109.5 |
N1—N2—H2 | 124.4 | C9—C12—H12B | 109.5 |
C3—N2—H2 | 124.4 | H12A—C12—H12B | 109.5 |
C7—N3—N4 | 105.4 (2) | C9—C12—H12C | 109.5 |
C7—N3—Cu1 | 131.45 (17) | H12A—C12—H12C | 109.5 |
N4—N3—Cu1 | 123.11 (15) | H12B—C12—H12C | 109.5 |
C9—N4—N3 | 111.5 (2) | N5—C13—C14 | 109.4 (2) |
C9—N4—H4 | 124.3 | N5—C13—C16 | 122.6 (2) |
N3—N4—H4 | 124.3 | C14—C13—C16 | 128.0 (2) |
C13—N5—N6 | 105.96 (18) | C15—C14—C13 | 106.0 (2) |
C13—N5—Cu1 | 133.56 (17) | C15—C14—C17 | 126.4 (3) |
N6—N5—Cu1 | 119.77 (14) | C13—C14—C17 | 127.6 (3) |
C15—N6—N5 | 111.9 (2) | N6—C15—C14 | 106.8 (2) |
C15—N6—H6 | 124.1 | N6—C15—C18 | 122.2 (2) |
N5—N6—H6 | 124.1 | C14—C15—C18 | 130.9 (2) |
N1—C1—C2 | 110.1 (2) | C13—C16—H16A | 109.5 |
N1—C1—C4 | 121.6 (2) | C13—C16—H16B | 109.5 |
C2—C1—C4 | 128.3 (2) | H16A—C16—H16B | 109.5 |
C3—C2—C1 | 105.7 (2) | C13—C16—H16C | 109.5 |
C3—C2—C5 | 127.1 (2) | H16A—C16—H16C | 109.5 |
C1—C2—C5 | 127.2 (2) | H16B—C16—H16C | 109.5 |
N2—C3—C2 | 107.3 (2) | C14—C17—H17A | 109.5 |
N2—C3—C6 | 121.4 (2) | C14—C17—H17B | 109.5 |
C2—C3—C6 | 131.4 (2) | H17A—C17—H17B | 109.5 |
C1—C4—H4A | 109.5 | C14—C17—H17C | 109.5 |
C1—C4—H4B | 109.5 | H17A—C17—H17C | 109.5 |
H4A—C4—H4B | 109.5 | H17B—C17—H17C | 109.5 |
C1—C4—H4C | 109.5 | C15—C18—H18A | 109.5 |
H4A—C4—H4C | 109.5 | C15—C18—H18B | 109.5 |
H4B—C4—H4C | 109.5 | H18A—C18—H18B | 109.5 |
C2—C5—H5A | 109.5 | C15—C18—H18C | 109.5 |
C2—C5—H5B | 109.5 | H18A—C18—H18C | 109.5 |
H5A—C5—H5B | 109.5 | H18B—C18—H18C | 109.5 |
F5—Nb1—O1—Cu1 | 134.6 (3) | N4—N3—C7—C10 | 179.4 (2) |
F4—Nb1—O1—Cu1 | 44.9 (4) | Cu1—N3—C7—C10 | −0.5 (3) |
F2—Nb1—O1—Cu1 | −134.5 (3) | N3—C7—C8—C9 | −0.2 (3) |
F3—Nb1—O1—Cu1 | −44.8 (4) | C10—C7—C8—C9 | −179.2 (2) |
C1—N1—N2—C3 | 0.4 (3) | N3—C7—C8—C11 | 178.1 (2) |
Cu1—N1—N2—C3 | −176.64 (16) | C10—C7—C8—C11 | −0.9 (4) |
C7—N3—N4—C9 | −0.4 (2) | N3—N4—C9—C8 | 0.3 (3) |
Cu1—N3—N4—C9 | 179.55 (15) | N3—N4—C9—C12 | −179.9 (2) |
C13—N5—N6—C15 | 0.0 (3) | C7—C8—C9—N4 | −0.1 (3) |
Cu1—N5—N6—C15 | −171.60 (16) | C11—C8—C9—N4 | −178.3 (3) |
N2—N1—C1—C2 | −0.5 (3) | C7—C8—C9—C12 | −179.9 (3) |
Cu1—N1—C1—C2 | 176.02 (17) | C11—C8—C9—C12 | 1.8 (5) |
N2—N1—C1—C4 | −179.5 (2) | N6—N5—C13—C14 | −0.8 (3) |
Cu1—N1—C1—C4 | −3.0 (4) | Cu1—N5—C13—C14 | 169.10 (17) |
N1—C1—C2—C3 | 0.4 (3) | N6—N5—C13—C16 | 177.0 (2) |
C4—C1—C2—C3 | 179.3 (3) | Cu1—N5—C13—C16 | −13.1 (4) |
N1—C1—C2—C5 | −179.2 (2) | N5—C13—C14—C15 | 1.3 (3) |
C4—C1—C2—C5 | −0.4 (4) | C16—C13—C14—C15 | −176.3 (3) |
N1—N2—C3—C2 | −0.1 (3) | N5—C13—C14—C17 | −176.8 (2) |
N1—N2—C3—C6 | −179.2 (3) | C16—C13—C14—C17 | 5.5 (4) |
C1—C2—C3—N2 | −0.2 (3) | N5—N6—C15—C14 | 0.8 (3) |
C5—C2—C3—N2 | 179.5 (2) | N5—N6—C15—C18 | −177.4 (2) |
C1—C2—C3—C6 | 178.8 (3) | C13—C14—C15—N6 | −1.3 (3) |
C5—C2—C3—C6 | −1.5 (5) | C17—C14—C15—N6 | 176.9 (2) |
N4—N3—C7—C8 | 0.4 (2) | C13—C14—C15—C18 | 176.7 (3) |
Cu1—N3—C7—C8 | −179.59 (16) | C17—C14—C15—C18 | −5.1 (5) |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (ii) −x, y+1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···F2i | 0.87 | 2.06 | 2.887 (3) | 159 |
N4—H4···F3i | 0.87 | 1.88 | 2.733 (3) | 165 |
N6—H6···F4i | 0.87 | 2.02 | 2.860 (2) | 161 |
C4—H4C···F5 | 0.97 | 2.62 | 3.449 (3) | 143 |
C10—H10A···F5iii | 0.97 | 2.47 | 3.334 (3) | 148 |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (iii) −x, −y+1, −z+1. |
[CuTaF5O(C6H10N2)3] | F(000) = 1340 |
Mr = 685.97 | Dx = 1.858 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 9.3367 (3) Å | Cell parameters from 8000 reflections |
b = 13.1541 (6) Å | θ = 2.6–27.9° |
c = 20.0036 (5) Å | µ = 5.38 mm−1 |
β = 93.232 (3)° | T = 213 K |
V = 2452.85 (15) Å3 | Prism, blue |
Z = 4 | 0.20 × 0.16 × 0.10 mm |
Stoe image plate diffraction system diffractometer | 4236 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.056 |
φ oscillation scans | θmax = 27.9°, θmin = 2.6° |
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)] | h = −11→12 |
Tmin = 0.361, Tmax = 0.547 | k = −17→17 |
20527 measured reflections | l = −25→24 |
5760 independent reflections |
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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.052 | H-atom parameters constrained |
S = 0.84 | w = 1/[σ2(Fo2) + (0.0237P)2] where P = (Fo2 + 2Fc2)/3 |
5760 reflections | (Δ/σ)max = 0.003 |
298 parameters | Δρmax = 1.38 e Å−3 |
0 restraints | Δρmin = −0.92 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
x | y | z | Uiso*/Ueq | ||
Ta1 | −0.01099 (2) | 0.55499 (2) | 0.28505 (2) | 0.02515 (5) | |
Cu1 | −0.05578 (5) | 0.30148 (3) | 0.35545 (2) | 0.02243 (9) | |
O1 | −0.0249 (3) | 0.44084 (17) | 0.33123 (13) | 0.0342 (6) | |
F1 | 0.0140 (2) | 0.68133 (13) | 0.22341 (11) | 0.0327 (5) | |
F2 | 0.1738 (2) | 0.59924 (15) | 0.32167 (12) | 0.0379 (5) | |
F3 | 0.0838 (3) | 0.49229 (15) | 0.21171 (12) | 0.0407 (6) | |
F4 | −0.1896 (2) | 0.54658 (15) | 0.23248 (11) | 0.0380 (5) | |
F5 | −0.1027 (3) | 0.64379 (16) | 0.34469 (12) | 0.0420 (6) | |
N1 | −0.2530 (3) | 0.31190 (19) | 0.31305 (15) | 0.0264 (7) | |
N2 | −0.2979 (4) | 0.2513 (2) | 0.26134 (16) | 0.0329 (7) | |
H2 | −0.2468 | 0.2027 | 0.2453 | 0.040* | |
N3 | −0.1136 (3) | 0.19329 (19) | 0.42046 (15) | 0.0262 (7) | |
N4 | −0.1384 (3) | 0.0949 (2) | 0.40310 (16) | 0.0301 (7) | |
H4 | −0.1321 | 0.0707 | 0.3629 | 0.036* | |
N5 | 0.1501 (3) | 0.28565 (19) | 0.38600 (15) | 0.0260 (6) | |
N6 | 0.2277 (3) | 0.2068 (2) | 0.36442 (16) | 0.0291 (7) | |
H6 | 0.1974 | 0.1647 | 0.3332 | 0.035* | |
C1 | −0.3620 (4) | 0.3757 (2) | 0.32148 (19) | 0.0269 (8) | |
C2 | −0.4755 (4) | 0.3556 (3) | 0.2753 (2) | 0.0322 (8) | |
C3 | −0.4308 (4) | 0.2753 (3) | 0.2379 (2) | 0.0361 (9) | |
C4 | −0.3525 (5) | 0.4564 (3) | 0.3736 (2) | 0.0410 (10) | |
H4A | −0.2799 | 0.4381 | 0.4081 | 0.062* | |
H4B | −0.4445 | 0.4634 | 0.3933 | 0.062* | |
H4C | −0.3268 | 0.5204 | 0.3533 | 0.062* | |
C5 | −0.6164 (5) | 0.4098 (3) | 0.2677 (2) | 0.0491 (11) | |
H5A | −0.6052 | 0.4716 | 0.2420 | 0.074* | |
H5B | −0.6486 | 0.4269 | 0.3116 | 0.074* | |
H5C | −0.6867 | 0.3662 | 0.2445 | 0.074* | |
C6 | −0.5063 (6) | 0.2184 (4) | 0.1816 (3) | 0.0678 (16) | |
H6A | −0.5830 | 0.1780 | 0.1987 | 0.102* | |
H6B | −0.4387 | 0.1741 | 0.1608 | 0.102* | |
H6C | −0.5462 | 0.2663 | 0.1487 | 0.102* | |
C7 | −0.1353 (4) | 0.1990 (3) | 0.48491 (19) | 0.0297 (8) | |
C8 | −0.1734 (5) | 0.1032 (3) | 0.5104 (2) | 0.0375 (9) | |
C9 | −0.1741 (4) | 0.0398 (3) | 0.4564 (2) | 0.0373 (9) | |
C10 | −0.1176 (5) | 0.2963 (3) | 0.5228 (2) | 0.0448 (11) | |
H10A | −0.0265 | 0.2958 | 0.5486 | 0.067* | |
H10B | −0.1951 | 0.3035 | 0.5528 | 0.067* | |
H10C | −0.1197 | 0.3528 | 0.4916 | 0.067* | |
C11 | −0.2041 (6) | 0.0790 (4) | 0.5812 (2) | 0.0633 (15) | |
H11A | −0.3029 | 0.0962 | 0.5888 | 0.095* | |
H11B | −0.1405 | 0.1181 | 0.6113 | 0.095* | |
H11C | −0.1888 | 0.0070 | 0.5893 | 0.095* | |
C12 | −0.2071 (6) | −0.0716 (3) | 0.4494 (3) | 0.0551 (13) | |
H12A | −0.1702 | −0.1072 | 0.4892 | 0.083* | |
H12B | −0.1624 | −0.0984 | 0.4105 | 0.083* | |
H12C | −0.3102 | −0.0811 | 0.4440 | 0.083* | |
C13 | 0.2347 (4) | 0.3303 (3) | 0.4336 (2) | 0.0334 (9) | |
C14 | 0.3635 (4) | 0.2787 (3) | 0.4424 (2) | 0.0348 (9) | |
C15 | 0.3565 (4) | 0.2011 (3) | 0.3966 (2) | 0.0330 (9) | |
C16 | 0.1892 (5) | 0.4250 (3) | 0.4686 (2) | 0.0507 (12) | |
H16A | 0.0994 | 0.4494 | 0.4477 | 0.076* | |
H16B | 0.2623 | 0.4769 | 0.4653 | 0.076* | |
H16C | 0.1766 | 0.4100 | 0.5154 | 0.076* | |
C17 | 0.4866 (5) | 0.2997 (4) | 0.4929 (3) | 0.0622 (14) | |
H17A | 0.4849 | 0.2508 | 0.5291 | 0.093* | |
H17B | 0.4773 | 0.3678 | 0.5107 | 0.093* | |
H17C | 0.5767 | 0.2940 | 0.4712 | 0.093* | |
C18 | 0.4665 (5) | 0.1228 (3) | 0.3803 (3) | 0.0493 (12) | |
H18A | 0.4269 | 0.0783 | 0.3453 | 0.074* | |
H18B | 0.4924 | 0.0831 | 0.4200 | 0.074* | |
H18C | 0.5511 | 0.1565 | 0.3651 | 0.074* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ta1 | 0.02802 (8) | 0.02028 (6) | 0.02680 (8) | −0.00233 (7) | −0.00164 (5) | 0.00654 (6) |
Cu1 | 0.0242 (2) | 0.01817 (16) | 0.0246 (2) | −0.00010 (16) | −0.00177 (17) | 0.00329 (15) |
O1 | 0.0369 (15) | 0.0234 (11) | 0.0416 (16) | −0.0039 (11) | −0.0034 (12) | 0.0128 (11) |
F1 | 0.0347 (12) | 0.0268 (9) | 0.0359 (14) | −0.0055 (9) | −0.0029 (10) | 0.0131 (8) |
F2 | 0.0314 (13) | 0.0362 (11) | 0.0447 (15) | −0.0076 (10) | −0.0101 (10) | 0.0122 (10) |
F3 | 0.0517 (16) | 0.0343 (11) | 0.0370 (14) | 0.0087 (11) | 0.0091 (11) | 0.0050 (9) |
F4 | 0.0319 (13) | 0.0364 (11) | 0.0445 (14) | −0.0077 (10) | −0.0085 (10) | 0.0107 (10) |
F5 | 0.0486 (16) | 0.0369 (11) | 0.0414 (15) | 0.0019 (11) | 0.0106 (11) | −0.0019 (10) |
N1 | 0.0257 (17) | 0.0228 (13) | 0.0301 (19) | 0.0029 (12) | −0.0033 (13) | 0.0001 (11) |
N2 | 0.0343 (19) | 0.0313 (15) | 0.032 (2) | 0.0067 (14) | −0.0064 (14) | −0.0091 (13) |
N3 | 0.0305 (18) | 0.0226 (13) | 0.0255 (19) | −0.0018 (12) | 0.0014 (13) | 0.0047 (12) |
N4 | 0.0347 (19) | 0.0235 (13) | 0.0323 (19) | −0.0014 (13) | 0.0028 (14) | 0.0022 (12) |
N5 | 0.0242 (16) | 0.0236 (13) | 0.0297 (18) | −0.0028 (12) | −0.0032 (13) | −0.0015 (12) |
N6 | 0.0281 (17) | 0.0236 (13) | 0.035 (2) | 0.0008 (13) | −0.0030 (13) | −0.0026 (12) |
C1 | 0.028 (2) | 0.0252 (15) | 0.027 (2) | 0.0022 (14) | 0.0034 (15) | 0.0035 (13) |
C2 | 0.027 (2) | 0.0360 (19) | 0.034 (2) | 0.0066 (16) | −0.0002 (16) | 0.0056 (16) |
C3 | 0.027 (2) | 0.043 (2) | 0.037 (2) | 0.0034 (17) | −0.0063 (17) | −0.0014 (17) |
C4 | 0.038 (2) | 0.036 (2) | 0.050 (3) | 0.0072 (18) | 0.0050 (19) | −0.0103 (18) |
C5 | 0.033 (2) | 0.057 (2) | 0.057 (3) | 0.012 (2) | −0.002 (2) | 0.001 (2) |
C6 | 0.055 (3) | 0.087 (4) | 0.058 (4) | 0.013 (3) | −0.023 (3) | −0.029 (3) |
C7 | 0.033 (2) | 0.0319 (17) | 0.024 (2) | 0.0015 (16) | −0.0021 (16) | 0.0033 (15) |
C8 | 0.042 (3) | 0.040 (2) | 0.031 (2) | −0.0030 (18) | 0.0052 (18) | 0.0125 (17) |
C9 | 0.033 (2) | 0.0306 (19) | 0.049 (3) | −0.0025 (16) | 0.0036 (18) | 0.0138 (17) |
C10 | 0.060 (3) | 0.046 (2) | 0.028 (3) | −0.003 (2) | 0.000 (2) | −0.0092 (18) |
C11 | 0.081 (4) | 0.071 (3) | 0.039 (3) | −0.005 (3) | 0.010 (3) | 0.022 (2) |
C12 | 0.064 (3) | 0.032 (2) | 0.071 (4) | −0.008 (2) | 0.010 (3) | 0.013 (2) |
C13 | 0.039 (2) | 0.0321 (18) | 0.029 (2) | −0.0081 (17) | −0.0010 (17) | −0.0001 (15) |
C14 | 0.031 (2) | 0.040 (2) | 0.032 (2) | −0.0097 (17) | −0.0078 (17) | 0.0087 (16) |
C15 | 0.023 (2) | 0.0341 (18) | 0.042 (3) | 0.0005 (16) | 0.0004 (16) | 0.0125 (17) |
C16 | 0.055 (3) | 0.046 (2) | 0.051 (3) | −0.007 (2) | −0.006 (2) | −0.020 (2) |
C17 | 0.050 (3) | 0.083 (3) | 0.050 (3) | −0.017 (3) | −0.025 (2) | 0.012 (3) |
C18 | 0.032 (2) | 0.048 (2) | 0.068 (3) | 0.0096 (19) | 0.004 (2) | 0.009 (2) |
Ta1—O1 | 1.771 (2) | C5—H5B | 0.9700 |
Ta1—F5 | 1.907 (2) | C5—H5C | 0.9700 |
Ta1—F4 | 1.924 (2) | C6—H6A | 0.9700 |
Ta1—F2 | 1.926 (2) | C6—H6B | 0.9700 |
Ta1—F3 | 1.940 (2) | C6—H6C | 0.9700 |
Ta1—F1 | 2.0904 (18) | C7—C8 | 1.413 (5) |
Cu1—O1 | 1.922 (2) | C7—C10 | 1.491 (5) |
Cu1—N1 | 1.988 (3) | C8—C9 | 1.364 (6) |
Cu1—N5 | 1.995 (3) | C8—C11 | 1.495 (6) |
Cu1—N3 | 2.022 (3) | C9—C12 | 1.502 (5) |
Cu1—F1i | 2.2820 (19) | C10—H10A | 0.9700 |
F1—Cu1ii | 2.2821 (19) | C10—H10B | 0.9700 |
N1—C1 | 1.337 (4) | C10—H10C | 0.9700 |
N1—N2 | 1.354 (4) | C11—H11A | 0.9700 |
N2—C3 | 1.339 (5) | C11—H11B | 0.9700 |
N2—H2 | 0.8700 | C11—H11C | 0.9700 |
N3—C7 | 1.318 (5) | C12—H12A | 0.9700 |
N3—N4 | 1.357 (4) | C12—H12B | 0.9700 |
N4—C9 | 1.346 (5) | C12—H12C | 0.9700 |
N4—H4 | 0.8700 | C13—C14 | 1.383 (6) |
N5—C13 | 1.338 (5) | C13—C16 | 1.503 (5) |
N5—N6 | 1.350 (4) | C14—C15 | 1.369 (6) |
N6—C15 | 1.334 (5) | C14—C17 | 1.513 (5) |
N6—H6 | 0.8700 | C15—C18 | 1.503 (5) |
C1—C2 | 1.391 (5) | C16—H16A | 0.9700 |
C1—C4 | 1.486 (5) | C16—H16B | 0.9700 |
C2—C3 | 1.372 (5) | C16—H16C | 0.9700 |
C2—C5 | 1.497 (5) | C17—H17A | 0.9700 |
C3—C6 | 1.496 (6) | C17—H17B | 0.9700 |
C4—H4A | 0.9700 | C17—H17C | 0.9700 |
C4—H4B | 0.9700 | C18—H18A | 0.9700 |
C4—H4C | 0.9700 | C18—H18B | 0.9700 |
C5—H5A | 0.9700 | C18—H18C | 0.9700 |
O1—Ta1—F5 | 98.30 (11) | C2—C5—H5C | 109.5 |
O1—Ta1—F4 | 98.59 (10) | H5A—C5—H5C | 109.5 |
F5—Ta1—F4 | 88.35 (10) | H5B—C5—H5C | 109.5 |
O1—Ta1—F2 | 98.53 (10) | C3—C6—H6A | 109.5 |
F5—Ta1—F2 | 90.06 (10) | C3—C6—H6B | 109.5 |
F4—Ta1—F2 | 162.85 (8) | H6A—C6—H6B | 109.5 |
O1—Ta1—F3 | 94.82 (11) | C3—C6—H6C | 109.5 |
F5—Ta1—F3 | 166.86 (9) | H6A—C6—H6C | 109.5 |
F4—Ta1—F3 | 88.89 (10) | H6B—C6—H6C | 109.5 |
F2—Ta1—F3 | 88.80 (10) | N3—C7—C8 | 110.9 (3) |
O1—Ta1—F1 | 174.50 (11) | N3—C7—C10 | 121.8 (3) |
F5—Ta1—F1 | 87.19 (9) | C8—C7—C10 | 127.3 (4) |
F4—Ta1—F1 | 81.11 (8) | C9—C8—C7 | 104.5 (3) |
F2—Ta1—F1 | 81.76 (8) | C9—C8—C11 | 128.9 (4) |
F3—Ta1—F1 | 79.69 (9) | C7—C8—C11 | 126.7 (4) |
O1—Cu1—N1 | 88.57 (11) | N4—C9—C8 | 107.9 (3) |
O1—Cu1—N5 | 91.22 (11) | N4—C9—C12 | 120.7 (4) |
N1—Cu1—N5 | 172.39 (13) | C8—C9—C12 | 131.4 (4) |
O1—Cu1—N3 | 151.99 (12) | C7—C10—H10A | 109.5 |
N1—Cu1—N3 | 92.78 (12) | C7—C10—H10B | 109.5 |
N5—Cu1—N3 | 90.98 (12) | H10A—C10—H10B | 109.5 |
O1—Cu1—F1i | 116.90 (10) | C7—C10—H10C | 109.5 |
N1—Cu1—F1i | 86.74 (10) | H10A—C10—H10C | 109.5 |
N5—Cu1—F1i | 86.57 (10) | H10B—C10—H10C | 109.5 |
N3—Cu1—F1i | 91.11 (10) | C8—C11—H11A | 109.5 |
Ta1—O1—Cu1 | 163.01 (16) | C8—C11—H11B | 109.5 |
Ta1—F1—Cu1ii | 170.94 (12) | H11A—C11—H11B | 109.5 |
C1—N1—N2 | 105.1 (3) | C8—C11—H11C | 109.5 |
C1—N1—Cu1 | 133.0 (2) | H11A—C11—H11C | 109.5 |
N2—N1—Cu1 | 121.7 (2) | H11B—C11—H11C | 109.5 |
C3—N2—N1 | 111.7 (3) | C9—C12—H12A | 109.5 |
C3—N2—H2 | 124.2 | C9—C12—H12B | 109.5 |
N1—N2—H2 | 124.2 | H12A—C12—H12B | 109.5 |
C7—N3—N4 | 105.8 (3) | C9—C12—H12C | 109.5 |
C7—N3—Cu1 | 130.5 (2) | H12A—C12—H12C | 109.5 |
N4—N3—Cu1 | 123.7 (2) | H12B—C12—H12C | 109.5 |
C9—N4—N3 | 110.9 (3) | N5—C13—C14 | 110.5 (3) |
C9—N4—H4 | 124.5 | N5—C13—C16 | 121.6 (4) |
N3—N4—H4 | 124.5 | C14—C13—C16 | 127.9 (4) |
C13—N5—N6 | 105.0 (3) | C15—C14—C13 | 105.8 (3) |
C13—N5—Cu1 | 133.8 (3) | C15—C14—C17 | 126.0 (4) |
N6—N5—Cu1 | 120.5 (2) | C13—C14—C17 | 128.2 (4) |
C15—N6—N5 | 112.0 (3) | N6—C15—C14 | 106.8 (3) |
C15—N6—H6 | 124.0 | N6—C15—C18 | 122.8 (4) |
N5—N6—H6 | 124.0 | C14—C15—C18 | 130.4 (4) |
N1—C1—C2 | 110.7 (3) | C13—C16—H16A | 109.5 |
N1—C1—C4 | 121.4 (3) | C13—C16—H16B | 109.5 |
C2—C1—C4 | 127.9 (3) | H16A—C16—H16B | 109.5 |
C3—C2—C1 | 105.4 (3) | C13—C16—H16C | 109.5 |
C3—C2—C5 | 127.1 (4) | H16A—C16—H16C | 109.5 |
C1—C2—C5 | 127.5 (4) | H16B—C16—H16C | 109.5 |
N2—C3—C2 | 107.2 (3) | C14—C17—H17A | 109.5 |
N2—C3—C6 | 122.2 (4) | C14—C17—H17B | 109.5 |
C2—C3—C6 | 130.6 (4) | H17A—C17—H17B | 109.5 |
C1—C4—H4A | 109.5 | C14—C17—H17C | 109.5 |
C1—C4—H4B | 109.5 | H17A—C17—H17C | 109.5 |
H4A—C4—H4B | 109.5 | H17B—C17—H17C | 109.5 |
C1—C4—H4C | 109.5 | C15—C18—H18A | 109.5 |
H4A—C4—H4C | 109.5 | C15—C18—H18B | 109.5 |
H4B—C4—H4C | 109.5 | H18A—C18—H18B | 109.5 |
C2—C5—H5A | 109.5 | C15—C18—H18C | 109.5 |
C2—C5—H5B | 109.5 | H18A—C18—H18C | 109.5 |
H5A—C5—H5B | 109.5 | H18B—C18—H18C | 109.5 |
F5—Ta1—O1—Cu1 | 136.5 (6) | N4—N3—C7—C10 | 179.7 (4) |
F4—Ta1—O1—Cu1 | 46.9 (6) | Cu1—N3—C7—C10 | −0.3 (6) |
F2—Ta1—O1—Cu1 | −132.2 (6) | N3—C7—C8—C9 | −0.5 (5) |
F3—Ta1—O1—Cu1 | −42.7 (6) | C10—C7—C8—C9 | −179.5 (4) |
C1—N1—N2—C3 | −0.3 (4) | N3—C7—C8—C11 | 179.0 (4) |
Cu1—N1—N2—C3 | −176.2 (3) | C10—C7—C8—C11 | −0.1 (7) |
C7—N3—N4—C9 | −0.5 (4) | N3—N4—C9—C8 | 0.2 (5) |
Cu1—N3—N4—C9 | 179.6 (3) | N3—N4—C9—C12 | 179.8 (4) |
C13—N5—N6—C15 | 0.0 (4) | C7—C8—C9—N4 | 0.1 (5) |
Cu1—N5—N6—C15 | −171.8 (2) | C11—C8—C9—N4 | −179.3 (5) |
N2—N1—C1—C2 | 0.0 (4) | C7—C8—C9—C12 | −179.4 (5) |
Cu1—N1—C1—C2 | 175.3 (3) | C11—C8—C9—C12 | 1.2 (9) |
N2—N1—C1—C4 | −178.9 (3) | N6—N5—C13—C14 | −1.0 (4) |
Cu1—N1—C1—C4 | −3.6 (5) | Cu1—N5—C13—C14 | 169.1 (3) |
N1—C1—C2—C3 | 0.2 (4) | N6—N5—C13—C16 | 177.4 (4) |
C4—C1—C2—C3 | 179.0 (4) | Cu1—N5—C13—C16 | −12.5 (6) |
N1—C1—C2—C5 | −179.6 (4) | N5—C13—C14—C15 | 1.6 (4) |
C4—C1—C2—C5 | −0.8 (7) | C16—C13—C14—C15 | −176.7 (4) |
N1—N2—C3—C2 | 0.4 (5) | N5—C13—C14—C17 | −176.8 (4) |
N1—N2—C3—C6 | −178.9 (4) | C16—C13—C14—C17 | 4.9 (7) |
C1—C2—C3—N2 | −0.4 (4) | N5—N6—C15—C14 | 1.0 (4) |
C5—C2—C3—N2 | 179.5 (4) | N5—N6—C15—C18 | −177.5 (3) |
C1—C2—C3—C6 | 178.9 (5) | C13—C14—C15—N6 | −1.6 (4) |
C5—C2—C3—C6 | −1.3 (8) | C17—C14—C15—N6 | 176.9 (4) |
N4—N3—C7—C8 | 0.6 (4) | C13—C14—C15—C18 | 176.8 (4) |
Cu1—N3—C7—C8 | −179.5 (3) | C17—C14—C15—C18 | −4.7 (7) |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (ii) −x, y+1/2, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···F2i | 0.87 | 2.05 | 2.884 (4) | 160 |
N4—H4···F3i | 0.87 | 1.89 | 2.736 (4) | 164 |
N6—H6···F4i | 0.87 | 2.03 | 2.872 (4) | 162 |
C4—H4C···F5 | 0.97 | 2.66 | 3.464 (5) | 140 |
C10—H10A···F5iii | 0.97 | 2.52 | 3.356 (5) | 144 |
Symmetry codes: (i) −x, y−1/2, −z+1/2; (iii) −x, −y+1, −z+1. |
Compound | Axial M—O/M—F bonds | Equatorial M—F bonds | ||||
Ordered anions | ||||||
[Cu(Me3pz)3{NbOF5}]n, (I) | 1.7479 (17) | 2.1134 (13) | 1.9008 (15) | 1.9298 (12) | 1.9306 (13) | 1.9487 (15) |
0.0031 (11) | 0.0008 (9) | 0.0018 (10) | 0.0007 (8) | 0.0001 (8) | 0.0021 (10) | |
[Cu(Me3pz)3{TaOF5}]n, (II) | 1.771 (2) | 2.0904 (18) | 1.907 (2) | 1.924 (2) | 1.926 (2) | 1.940 (2) |
0.0007 (13) | 0.0008 (11) | 0.0004 (15) | 0.0013 (13) | 0.0005 (13) | 0.0005 (14) | |
Disordered anionsa | ||||||
[Cu(pz)4{NbOF5}]nb | 1.923 (3) ×2f | 1.927 (3) ×2 | 1.928 (3) ×2 | |||
0.023 (2) | 0.001 (2) | 0.0092 (17) | ||||
[Cd(py)4{NbOF5}]n, (A)c | 1.8841 (19) | 1.9619 (19) | 1.901 (2) | 1.909 (2) | 1.911 (2) | 1.913 (2) |
0.0324 (13) | 0.0129 (14) | 0.0035 (16) | 0.0008 (16) | 0.0002 (17) | 0.0007 (17) | |
[Cd(py)4{NbOF5}]n, (B)c | 1.925 (2) ×2f | 1.902 (2) ×2 | 1.930 (2) ×2 | |||
0.0260 (9) | 0.0009 (9) | 0.0007 (8) | ||||
[Cd(3-apy)4{NbOF5}]nd | 1.914 (3) | 1.937 (3) | 1.905 (4) | 1.912 (4) | 1.913 (3) | 1.930 (4) |
0.0286 (12) | 0.0172 (13) | 0.005 (2) | 0.003 (2) | 0.001 (2) | 0.004 (2) | |
[Cu(py)4{TaOF5}]ne | 1.924 (3) ×2 f) | 1.908 (3) ×2 | 1.923 (3) ×2 | |||
0.0199 (12) | 0.0054 (19) | 0.0034 (18) |
Notes: (a) pz = pyrazole, py = pyridine and 3-apy = 3-aminopyridine. The differences of the ADPs are calculated with anisotropic displacement parameters taken from the supplementary publications of (b) Mahenthirarajah et al. (2009), (c) Guillory et al. (2006) (A is the P21/c polymorph and B is the C2/c polymorph), (d) Izumi et al. (2005); (e) Norquist et al. (1998) and (f) the Nb (Ta) atoms reside on a crystallographically imposed centre of inversion. |
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