Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229620002594/ep3002sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229620002594/ep3002Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229620002594/ep3002IIsup3.hkl |
CCDC references: 1986082; 1986081
For both structures, data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
[Cd2(NO3)4(C14H14N4)3] | Z = 1 |
Mr = 1187.72 | F(000) = 598 |
Triclinic, P1 | Dx = 1.647 Mg m−3 |
a = 9.9336 (8) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.3115 (10) Å | Cell parameters from 3703 reflections |
c = 12.1571 (11) Å | θ = 3.9–28.5° |
α = 98.729 (8)° | µ = 0.97 mm−1 |
β = 101.515 (7)° | T = 293 K |
γ = 94.942 (7)° | Block, colourless |
V = 1197.31 (19) Å3 | 0.25 × 0.22 × 0.15 mm |
Rigaku Mercury CCD diffractometer | 5498 independent reflections |
Radiation source: fine-focus sealed tube | 4527 reflections with I > 2σ(I) |
Detector resolution: 28.5714 pixels mm-1 | Rint = 0.028 |
Graphite Monochromator scans | θmax = 29.5°, θmin = 3.5° |
Absorption correction: multi-scan (REQAB; Jacobson, 1998) | h = −9→12 |
Tmin = 0.780, Tmax = 1.000 | k = −12→13 |
10076 measured reflections | l = −16→16 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0289P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
5498 reflections | Δρmax = 0.36 e Å−3 |
325 parameters | Δρmin = −0.53 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 | ||
Cd1 | 0.02489 (2) | 0.75236 (2) | 0.24022 (2) | 0.04331 (8) | |
O1 | 0.0036 (3) | 0.9793 (2) | 0.34675 (18) | 0.0688 (6) | |
O2 | 0.2029 (3) | 0.9436 (2) | 0.3217 (2) | 0.0803 (7) | |
O3 | 0.2210 (2) | 0.6904 (2) | 0.16238 (19) | 0.0686 (6) | |
O4 | 0.0572 (3) | 0.5348 (2) | 0.14411 (19) | 0.0712 (6) | |
O5 | 0.1688 (3) | 1.1387 (2) | 0.39597 (19) | 0.0864 (8) | |
O6 | 0.2441 (3) | 0.4946 (2) | 0.0862 (2) | 0.1019 (9) | |
N1 | 0.0954 (2) | 0.6770 (2) | 0.40504 (18) | 0.0460 (5) | |
N2 | 0.1389 (2) | 0.6716 (2) | 0.58797 (17) | 0.0437 (5) | |
N3 | −0.0487 (2) | 0.8305 (2) | 0.07670 (17) | 0.0431 (5) | |
N4 | −0.1947 (2) | 0.9195 (2) | −0.04090 (17) | 0.0444 (5) | |
N5 | −0.2041 (2) | 0.7059 (2) | 0.24472 (18) | 0.0447 (5) | |
N6 | −0.3986 (2) | 0.71194 (18) | 0.30249 (17) | 0.0408 (5) | |
C1 | 0.0923 (3) | 0.7403 (3) | 0.5072 (2) | 0.0464 (6) | |
H1A | 0.0613 | 0.8226 | 0.5210 | 0.056* | |
C2 | 0.1461 (3) | 0.5617 (3) | 0.4237 (2) | 0.0496 (7) | |
H2A | 0.1594 | 0.4955 | 0.3672 | 0.060* | |
C3 | 0.1738 (3) | 0.5581 (3) | 0.5351 (2) | 0.0514 (7) | |
H3A | 0.2101 | 0.4906 | 0.5698 | 0.062* | |
C4 | 0.1558 (3) | 0.7153 (3) | 0.7105 (2) | 0.0547 (7) | |
H4A | 0.1404 | 0.6392 | 0.7464 | 0.066* | |
H4B | 0.0869 | 0.7735 | 0.7239 | 0.066* | |
C5 | 0.2975 (3) | 0.7869 (2) | 0.7641 (2) | 0.0453 (6) | |
C6 | 0.3866 (3) | 0.7384 (3) | 0.8453 (2) | 0.0624 (8) | |
H6A | 0.3592 | 0.6593 | 0.8672 | 0.075* | |
C7 | 0.5158 (3) | 0.8050 (3) | 0.8949 (3) | 0.0649 (9) | |
H7A | 0.5735 | 0.7708 | 0.9507 | 0.078* | |
C8 | 0.5615 (3) | 0.9209 (2) | 0.8638 (2) | 0.0438 (6) | |
C9 | 0.4722 (3) | 0.9679 (3) | 0.7816 (2) | 0.0596 (8) | |
H9A | 0.5001 | 1.0458 | 0.7582 | 0.072* | |
C10 | 0.3429 (3) | 0.9025 (3) | 0.7333 (3) | 0.0639 (8) | |
H10A | 0.2846 | 0.9374 | 0.6783 | 0.077* | |
C11 | 0.6980 (3) | 0.9999 (3) | 0.9186 (2) | 0.0542 (7) | |
H11A | 0.7284 | 1.0489 | 0.8641 | 0.065* | |
H11B | 0.6863 | 1.0635 | 0.9825 | 0.065* | |
C12 | −0.1409 (3) | 0.9133 (3) | 0.0667 (2) | 0.0465 (6) | |
H12A | −0.1659 | 0.9626 | 0.1284 | 0.056* | |
C13 | −0.1325 (3) | 0.8338 (3) | −0.1053 (2) | 0.0582 (8) | |
H13A | −0.1487 | 0.8162 | −0.1844 | 0.070* | |
C14 | −0.0435 (3) | 0.7796 (3) | −0.0327 (2) | 0.0501 (7) | |
H14A | 0.0130 | 0.7171 | −0.0535 | 0.060* | |
C15 | −0.2613 (3) | 0.7414 (2) | 0.3318 (2) | 0.0411 (6) | |
H15A | −0.2125 | 0.7816 | 0.4041 | 0.049* | |
C16 | −0.3107 (3) | 0.6514 (2) | 0.1561 (2) | 0.0488 (7) | |
H16A | −0.3019 | 0.6177 | 0.0828 | 0.059* | |
C17 | −0.4310 (3) | 0.6537 (2) | 0.1911 (2) | 0.0500 (7) | |
H17A | −0.5190 | 0.6218 | 0.1476 | 0.060* | |
C18 | −0.4922 (3) | 0.7248 (3) | 0.3822 (2) | 0.0517 (7) | |
H18A | −0.5846 | 0.7316 | 0.3406 | 0.062* | |
H18B | −0.4612 | 0.8051 | 0.4379 | 0.062* | |
C19 | −0.4963 (3) | 0.6073 (2) | 0.4432 (2) | 0.0426 (6) | |
C20 | −0.5375 (3) | 0.4812 (2) | 0.3833 (2) | 0.0463 (6) | |
H20A | −0.5629 | 0.4675 | 0.3041 | 0.056* | |
C21 | −0.4585 (3) | 0.6256 (2) | 0.5603 (2) | 0.0473 (7) | |
H21A | −0.4301 | 0.7103 | 0.6018 | 0.057* | |
N7 | 0.1256 (3) | 1.0219 (2) | 0.35643 (18) | 0.0568 (6) | |
N8 | 0.1749 (3) | 0.5723 (3) | 0.1292 (2) | 0.0596 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.03512 (13) | 0.05554 (14) | 0.04043 (12) | 0.00531 (9) | 0.00949 (9) | 0.01026 (8) |
O1 | 0.0626 (17) | 0.0659 (13) | 0.0714 (15) | −0.0001 (11) | 0.0104 (13) | 0.0012 (10) |
O2 | 0.0732 (19) | 0.0791 (15) | 0.0903 (17) | 0.0066 (13) | 0.0281 (15) | 0.0072 (12) |
O3 | 0.0515 (15) | 0.0641 (13) | 0.0860 (16) | 0.0066 (11) | 0.0150 (12) | 0.0004 (11) |
O4 | 0.0600 (16) | 0.0713 (13) | 0.0774 (16) | −0.0004 (11) | 0.0267 (13) | −0.0135 (11) |
O5 | 0.107 (2) | 0.0666 (14) | 0.0734 (16) | −0.0245 (13) | 0.0262 (15) | −0.0148 (11) |
O6 | 0.072 (2) | 0.0993 (18) | 0.124 (2) | 0.0131 (14) | 0.0396 (17) | −0.0393 (16) |
N1 | 0.0432 (15) | 0.0518 (13) | 0.0423 (13) | 0.0090 (10) | 0.0041 (10) | 0.0105 (10) |
N2 | 0.0354 (13) | 0.0511 (13) | 0.0420 (12) | 0.0024 (10) | 0.0007 (10) | 0.0119 (10) |
N3 | 0.0399 (14) | 0.0489 (12) | 0.0403 (12) | 0.0015 (10) | 0.0098 (10) | 0.0076 (9) |
N4 | 0.0427 (14) | 0.0453 (12) | 0.0410 (13) | −0.0030 (10) | 0.0022 (10) | 0.0087 (9) |
N5 | 0.0384 (14) | 0.0565 (13) | 0.0415 (12) | 0.0023 (10) | 0.0120 (10) | 0.0129 (10) |
N6 | 0.0382 (13) | 0.0471 (12) | 0.0423 (12) | 0.0048 (9) | 0.0137 (10) | 0.0174 (9) |
C1 | 0.0438 (17) | 0.0511 (15) | 0.0419 (15) | 0.0108 (12) | 0.0013 (12) | 0.0087 (11) |
C2 | 0.0388 (17) | 0.0502 (16) | 0.0592 (18) | 0.0108 (12) | 0.0095 (14) | 0.0059 (12) |
C3 | 0.0391 (17) | 0.0511 (17) | 0.0654 (19) | 0.0109 (13) | 0.0048 (14) | 0.0203 (14) |
C4 | 0.0432 (18) | 0.0751 (19) | 0.0444 (16) | 0.0004 (14) | 0.0054 (13) | 0.0155 (13) |
C5 | 0.0435 (17) | 0.0547 (15) | 0.0352 (14) | 0.0022 (12) | 0.0032 (12) | 0.0098 (11) |
C6 | 0.057 (2) | 0.0630 (18) | 0.0610 (19) | −0.0112 (15) | −0.0100 (15) | 0.0313 (14) |
C7 | 0.057 (2) | 0.0687 (19) | 0.0613 (19) | −0.0073 (15) | −0.0166 (16) | 0.0345 (15) |
C8 | 0.0439 (17) | 0.0457 (14) | 0.0399 (14) | 0.0026 (12) | 0.0024 (12) | 0.0120 (11) |
C9 | 0.061 (2) | 0.0542 (16) | 0.0596 (19) | −0.0010 (14) | −0.0079 (15) | 0.0297 (14) |
C10 | 0.058 (2) | 0.0698 (19) | 0.0604 (19) | 0.0052 (16) | −0.0074 (16) | 0.0296 (15) |
C11 | 0.0500 (19) | 0.0485 (15) | 0.0598 (18) | 0.0003 (13) | −0.0024 (14) | 0.0178 (13) |
C12 | 0.0465 (18) | 0.0509 (15) | 0.0405 (15) | 0.0065 (12) | 0.0069 (13) | 0.0063 (11) |
C13 | 0.071 (2) | 0.0645 (18) | 0.0382 (16) | 0.0038 (16) | 0.0151 (15) | 0.0057 (13) |
C14 | 0.054 (2) | 0.0557 (16) | 0.0442 (16) | 0.0096 (13) | 0.0182 (14) | 0.0089 (12) |
C15 | 0.0361 (16) | 0.0514 (15) | 0.0366 (14) | 0.0009 (11) | 0.0077 (11) | 0.0124 (11) |
C16 | 0.0495 (19) | 0.0576 (16) | 0.0383 (15) | −0.0019 (13) | 0.0109 (13) | 0.0080 (12) |
C17 | 0.0387 (17) | 0.0629 (17) | 0.0451 (16) | −0.0047 (13) | 0.0023 (13) | 0.0146 (12) |
C18 | 0.0497 (19) | 0.0575 (16) | 0.0601 (18) | 0.0158 (13) | 0.0273 (15) | 0.0225 (13) |
C19 | 0.0349 (16) | 0.0511 (15) | 0.0497 (16) | 0.0069 (11) | 0.0212 (12) | 0.0162 (12) |
C20 | 0.0442 (18) | 0.0573 (16) | 0.0410 (14) | 0.0033 (12) | 0.0172 (13) | 0.0102 (12) |
C21 | 0.0452 (18) | 0.0476 (15) | 0.0507 (16) | −0.0013 (12) | 0.0189 (13) | 0.0062 (12) |
N7 | 0.075 (2) | 0.0567 (16) | 0.0356 (13) | −0.0016 (14) | 0.0134 (13) | 0.0029 (10) |
N8 | 0.0469 (17) | 0.0759 (18) | 0.0505 (15) | 0.0119 (14) | 0.0104 (13) | −0.0089 (12) |
Cd1—N1 | 2.261 (2) | C4—H4A | 0.9700 |
Cd1—N3 | 2.268 (2) | C4—H4B | 0.9700 |
Cd1—N5 | 2.297 (2) | C5—C6 | 1.373 (4) |
Cd1—O3 | 2.422 (2) | C5—C10 | 1.369 (4) |
Cd1—O4 | 2.446 (2) | C6—C7 | 1.378 (4) |
Cd1—O2 | 2.471 (2) | C6—H6A | 0.9300 |
Cd1—O1 | 2.544 (2) | C7—C8 | 1.374 (3) |
O1—N7 | 1.230 (3) | C7—H7A | 0.9300 |
O2—N7 | 1.245 (3) | C8—C9 | 1.374 (3) |
O3—N8 | 1.240 (3) | C8—C11 | 1.493 (4) |
O4—N8 | 1.256 (3) | C9—C10 | 1.371 (4) |
O5—N7 | 1.232 (3) | C9—H9A | 0.9300 |
O6—N8 | 1.224 (3) | C10—H10A | 0.9300 |
N1—C1 | 1.320 (3) | C11—N4ii | 1.460 (3) |
N1—C2 | 1.363 (3) | C11—H11A | 0.9700 |
N2—C1 | 1.329 (3) | C11—H11B | 0.9700 |
N2—C3 | 1.354 (3) | C12—H12A | 0.9300 |
N2—C4 | 1.461 (3) | C13—C14 | 1.340 (4) |
N3—C12 | 1.305 (3) | C13—H13A | 0.9300 |
N3—C14 | 1.366 (3) | C14—H14A | 0.9300 |
N4—C12 | 1.324 (3) | C15—H15A | 0.9300 |
N4—C13 | 1.361 (3) | C16—C17 | 1.347 (4) |
N4—C11i | 1.460 (3) | C16—H16A | 0.9300 |
N5—C15 | 1.318 (3) | C17—H17A | 0.9300 |
N5—C16 | 1.363 (3) | C18—C19 | 1.515 (3) |
N6—C15 | 1.334 (3) | C18—H18A | 0.9700 |
N6—C17 | 1.357 (3) | C18—H18B | 0.9700 |
N6—C18 | 1.471 (3) | C19—C21 | 1.377 (3) |
C1—H1A | 0.9300 | C19—C20 | 1.376 (3) |
C2—C3 | 1.334 (4) | C20—C21iii | 1.385 (3) |
C2—H2A | 0.9300 | C20—H20A | 0.9300 |
C3—H3A | 0.9300 | C21—C20iii | 1.385 (3) |
C4—C5 | 1.503 (4) | C21—H21A | 0.9300 |
N1—Cd1—N3 | 178.82 (7) | C5—C6—C7 | 121.0 (3) |
N1—Cd1—N5 | 91.99 (8) | C5—C6—H6A | 119.5 |
N3—Cd1—N5 | 87.24 (8) | C7—C6—H6A | 119.5 |
N1—Cd1—O3 | 94.51 (8) | C8—C7—C6 | 121.5 (3) |
N3—Cd1—O3 | 86.61 (8) | C8—C7—H7A | 119.2 |
N5—Cd1—O3 | 148.37 (8) | C6—C7—H7A | 119.2 |
N1—Cd1—O4 | 86.24 (8) | C9—C8—C7 | 117.1 (3) |
N3—Cd1—O4 | 94.75 (8) | C9—C8—C11 | 119.3 (2) |
N5—Cd1—O4 | 97.63 (8) | C7—C8—C11 | 123.5 (2) |
O3—Cd1—O4 | 52.11 (7) | C10—C9—C8 | 121.4 (3) |
N1—Cd1—O2 | 86.29 (8) | C10—C9—H9A | 119.3 |
N3—Cd1—O2 | 93.60 (8) | C8—C9—H9A | 119.3 |
N5—Cd1—O2 | 134.34 (8) | C5—C10—C9 | 121.4 (3) |
O3—Cd1—O2 | 77.04 (8) | C5—C10—H10A | 119.3 |
O4—Cd1—O2 | 127.67 (8) | C9—C10—H10A | 119.3 |
N1—Cd1—O1 | 91.81 (7) | N4ii—C11—C8 | 113.4 (2) |
N3—Cd1—O1 | 87.23 (7) | N4ii—C11—H11A | 108.9 |
N5—Cd1—O1 | 84.64 (8) | C8—C11—H11A | 108.9 |
O3—Cd1—O1 | 125.96 (8) | N4ii—C11—H11B | 108.9 |
O4—Cd1—O1 | 177.05 (8) | C8—C11—H11B | 108.9 |
O2—Cd1—O1 | 49.90 (8) | H11A—C11—H11B | 107.7 |
N7—O1—Cd1 | 94.61 (17) | N3—C12—N4 | 112.7 (2) |
N7—O2—Cd1 | 97.78 (19) | N3—C12—H12A | 123.6 |
N8—O3—Cd1 | 95.77 (17) | N4—C12—H12A | 123.6 |
N8—O4—Cd1 | 94.20 (16) | C14—C13—N4 | 106.8 (2) |
C1—N1—C2 | 104.9 (2) | C14—C13—H13A | 126.6 |
C1—N1—Cd1 | 124.85 (17) | N4—C13—H13A | 126.6 |
C2—N1—Cd1 | 130.24 (18) | C13—C14—N3 | 109.5 (3) |
C1—N2—C3 | 106.9 (2) | C13—C14—H14A | 125.3 |
C1—N2—C4 | 125.8 (2) | N3—C14—H14A | 125.3 |
C3—N2—C4 | 127.3 (2) | N5—C15—N6 | 111.1 (2) |
C12—N3—C14 | 104.8 (2) | N5—C15—H15A | 124.5 |
C12—N3—Cd1 | 122.92 (17) | N6—C15—H15A | 124.5 |
C14—N3—Cd1 | 129.68 (18) | C17—C16—N5 | 109.5 (2) |
C12—N4—C13 | 106.2 (2) | C17—C16—H16A | 125.3 |
C12—N4—C11i | 126.5 (2) | N5—C16—H16A | 125.3 |
C13—N4—C11i | 127.3 (2) | C16—C17—N6 | 106.5 (3) |
C15—N5—C16 | 105.7 (2) | C16—C17—H17A | 126.8 |
C15—N5—Cd1 | 126.16 (18) | N6—C17—H17A | 126.8 |
C16—N5—Cd1 | 127.74 (17) | N6—C18—C19 | 111.3 (2) |
C15—N6—C17 | 107.3 (2) | N6—C18—H18A | 109.4 |
C15—N6—C18 | 124.9 (2) | C19—C18—H18A | 109.4 |
C17—N6—C18 | 127.3 (2) | N6—C18—H18B | 109.4 |
N1—C1—N2 | 111.5 (2) | C19—C18—H18B | 109.4 |
N1—C1—H1A | 124.3 | H18A—C18—H18B | 108.0 |
N2—C1—H1A | 124.3 | C21—C19—C20 | 118.9 (2) |
C3—C2—N1 | 109.8 (2) | C21—C19—C18 | 120.2 (2) |
C3—C2—H2A | 125.1 | C20—C19—C18 | 120.9 (2) |
N1—C2—H2A | 125.1 | C19—C20—C21iii | 120.6 (2) |
C2—C3—N2 | 106.9 (2) | C19—C20—H20A | 119.7 |
C2—C3—H3A | 126.5 | C21iii—C20—H20A | 119.7 |
N2—C3—H3A | 126.5 | C19—C21—C20iii | 120.6 (2) |
N2—C4—C5 | 112.0 (2) | C19—C21—H21A | 119.7 |
N2—C4—H4A | 109.2 | C20iii—C21—H21A | 119.7 |
C5—C4—H4A | 109.2 | O1—N7—O5 | 121.1 (3) |
N2—C4—H4B | 109.2 | O1—N7—O2 | 117.5 (2) |
C5—C4—H4B | 109.2 | O5—N7—O2 | 121.3 (3) |
H4A—C4—H4B | 107.9 | O6—N8—O3 | 120.7 (3) |
C6—C5—C10 | 117.6 (3) | O6—N8—O4 | 121.4 (3) |
C6—C5—C4 | 121.2 (2) | O3—N8—O4 | 117.9 (2) |
C10—C5—C4 | 121.2 (2) | ||
C2—N1—C1—N2 | 0.5 (3) | C11i—N4—C13—C14 | −178.5 (3) |
Cd1—N1—C1—N2 | 179.41 (17) | N4—C13—C14—N3 | −0.1 (3) |
C3—N2—C1—N1 | −0.1 (3) | C12—N3—C14—C13 | 0.2 (3) |
C4—N2—C1—N1 | 176.8 (2) | Cd1—N3—C14—C13 | 162.0 (2) |
C1—N1—C2—C3 | −0.7 (3) | C16—N5—C15—N6 | 0.0 (3) |
Cd1—N1—C2—C3 | −179.56 (19) | Cd1—N5—C15—N6 | 172.91 (14) |
N1—C2—C3—N2 | 0.7 (3) | C17—N6—C15—N5 | 0.5 (3) |
C1—N2—C3—C2 | −0.4 (3) | C18—N6—C15—N5 | 172.9 (2) |
C4—N2—C3—C2 | −177.2 (3) | C15—N5—C16—C17 | −0.4 (3) |
C1—N2—C4—C5 | −90.5 (3) | Cd1—N5—C16—C17 | −173.21 (16) |
C3—N2—C4—C5 | 85.8 (3) | N5—C16—C17—N6 | 0.7 (3) |
N2—C4—C5—C6 | −117.2 (3) | C15—N6—C17—C16 | −0.7 (3) |
N2—C4—C5—C10 | 62.4 (4) | C18—N6—C17—C16 | −172.9 (2) |
C10—C5—C6—C7 | 1.0 (5) | C15—N6—C18—C19 | −81.2 (3) |
C4—C5—C6—C7 | −179.4 (3) | C17—N6—C18—C19 | 89.7 (3) |
C5—C6—C7—C8 | −1.2 (5) | N6—C18—C19—C21 | 120.7 (3) |
C6—C7—C8—C9 | 0.4 (5) | N6—C18—C19—C20 | −59.3 (3) |
C6—C7—C8—C11 | 177.1 (3) | C21—C19—C20—C21iii | 0.3 (4) |
C7—C8—C9—C10 | 0.4 (5) | C18—C19—C20—C21iii | −179.7 (2) |
C11—C8—C9—C10 | −176.4 (3) | C20—C19—C21—C20iii | −0.3 (4) |
C6—C5—C10—C9 | −0.2 (5) | C18—C19—C21—C20iii | 179.7 (2) |
C4—C5—C10—C9 | −179.8 (3) | Cd1—O1—N7—O5 | 173.5 (2) |
C8—C9—C10—C5 | −0.6 (5) | Cd1—O1—N7—O2 | −4.4 (3) |
C9—C8—C11—N4ii | −152.1 (3) | Cd1—O2—N7—O1 | 4.6 (3) |
C7—C8—C11—N4ii | 31.3 (4) | Cd1—O2—N7—O5 | −173.4 (2) |
C14—N3—C12—N4 | −0.1 (3) | Cd1—O3—N8—O6 | −176.5 (2) |
Cd1—N3—C12—N4 | −163.57 (17) | Cd1—O3—N8—O4 | 1.5 (3) |
C13—N4—C12—N3 | 0.1 (3) | Cd1—O4—N8—O6 | 176.5 (3) |
C11i—N4—C12—N3 | 178.6 (2) | Cd1—O4—N8—O3 | −1.5 (3) |
C12—N4—C13—C14 | 0.0 (3) |
Symmetry codes: (i) x−1, y, z−1; (ii) x+1, y, z+1; (iii) −x−1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C15—H15A···O5iv | 0.93 | 2.38 | 3.267 (3) | 159 |
C16—H16A···O6v | 0.93 | 2.40 | 3.314 (4) | 168 |
C17—H17A···O6vi | 0.93 | 2.51 | 3.398 (4) | 160 |
Symmetry codes: (iv) −x, −y+2, −z+1; (v) −x, −y+1, −z; (vi) x−1, y, z. |
[Cd(C18H18N6)2](SiF6) | Dx = 1.521 Mg m−3 |
Mr = 891.26 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3 | Cell parameters from 3551 reflections |
a = 9.5898 (2) Å | θ = 4.1–29.1° |
c = 12.2158 (3) Å | µ = 0.67 mm−1 |
V = 972.91 (5) Å3 | T = 293 K |
Z = 1 | Block, colourless |
F(000) = 452 | 0.25 × 0.20 × 0.16 mm |
Rigaku Mercury CCD diffractometer | 1623 independent reflections |
Radiation source: fine-focus sealed tube | 1453 reflections with I > 2σ(I) |
Detector resolution: 28.5714 pixels mm-1 | Rint = 0.022 |
Graphite Monochromator scans | θmax = 29.3°, θmin = 4.1° |
Absorption correction: multi-scan (REQAB; Jacobson, 1998) | h = −13→12 |
Tmin = 0.882, Tmax = 1.000 | k = −12→12 |
8201 measured reflections | l = −15→16 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.027 | H-atom parameters constrained |
wR(F2) = 0.066 | w = 1/[σ2(Fo2) + (0.0287P)2 + 0.3052P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max < 0.001 |
1623 reflections | Δρmax = 0.26 e Å−3 |
86 parameters | Δρmin = −0.35 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 | ||
Cd1 | 1.0000 | 0.0000 | 0.5000 | 0.04031 (11) | |
Si1 | 0.0000 | 0.0000 | 0.0000 | 0.0305 (2) | |
F1 | 0.15248 (12) | 0.01996 (13) | 0.07938 (8) | 0.0457 (3) | |
N2 | 1.03296 (17) | 0.36519 (17) | 0.74645 (11) | 0.0389 (3) | |
C5 | 0.8255 (2) | 0.3663 (2) | 0.86320 (13) | 0.0378 (4) | |
N1 | 1.03700 (19) | 0.22129 (19) | 0.60726 (11) | 0.0446 (3) | |
C4 | 0.9968 (2) | 0.3999 (2) | 0.85695 (15) | 0.0437 (4) | |
H4A | 1.0702 | 0.5119 | 0.8748 | 0.052* | |
H4B | 1.0124 | 0.3336 | 0.9100 | 0.052* | |
C2 | 1.0838 (3) | 0.3742 (2) | 0.57260 (16) | 0.0533 (5) | |
H2A | 1.1135 | 0.4113 | 0.5013 | 0.064* | |
C6 | 0.6985 (2) | 0.2079 (2) | 0.86363 (14) | 0.0395 (4) | |
H6A | 0.7202 | 0.1236 | 0.8642 | 0.047* | |
C1 | 1.0070 (2) | 0.2215 (2) | 0.71248 (13) | 0.0433 (4) | |
H1A | 0.9718 | 0.1322 | 0.7578 | 0.052* | |
C3 | 1.0806 (2) | 0.4629 (2) | 0.65679 (18) | 0.0536 (5) | |
H3A | 1.1059 | 0.5700 | 0.6543 | 0.064* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.04950 (14) | 0.04950 (14) | 0.02193 (14) | 0.02475 (7) | 0.000 | 0.000 |
Si1 | 0.0354 (3) | 0.0354 (3) | 0.0208 (4) | 0.01768 (16) | 0.000 | 0.000 |
F1 | 0.0468 (6) | 0.0531 (6) | 0.0391 (5) | 0.0264 (5) | −0.0117 (4) | −0.0019 (4) |
N2 | 0.0355 (7) | 0.0412 (7) | 0.0392 (7) | 0.0186 (6) | −0.0046 (6) | −0.0062 (6) |
C5 | 0.0394 (9) | 0.0442 (9) | 0.0310 (7) | 0.0216 (7) | −0.0062 (6) | −0.0088 (7) |
N1 | 0.0571 (9) | 0.0504 (9) | 0.0300 (7) | 0.0298 (8) | −0.0006 (6) | 0.0006 (6) |
C4 | 0.0411 (9) | 0.0499 (10) | 0.0412 (9) | 0.0237 (8) | −0.0116 (7) | −0.0170 (8) |
C2 | 0.0623 (12) | 0.0536 (11) | 0.0424 (10) | 0.0278 (10) | 0.0094 (9) | 0.0117 (8) |
C6 | 0.0458 (9) | 0.0404 (9) | 0.0365 (8) | 0.0247 (8) | −0.0079 (7) | −0.0022 (7) |
C1 | 0.0592 (11) | 0.0447 (9) | 0.0308 (8) | 0.0297 (9) | −0.0025 (7) | −0.0003 (7) |
C3 | 0.0536 (11) | 0.0403 (10) | 0.0623 (12) | 0.0200 (9) | 0.0097 (9) | 0.0076 (9) |
Cd1—N1i | 2.3650 (15) | N2—C4 | 1.472 (2) |
Cd1—N1ii | 2.3650 (15) | C5—C6xi | 1.380 (2) |
Cd1—N1iii | 2.3650 (15) | C5—C6 | 1.394 (2) |
Cd1—N1 | 2.3650 (15) | C5—C4 | 1.510 (2) |
Cd1—N1iv | 2.3651 (15) | N1—C1 | 1.317 (2) |
Cd1—N1v | 2.3651 (15) | N1—C2 | 1.368 (2) |
Si1—F1 | 1.6838 (9) | C4—H4A | 0.9700 |
Si1—F1vi | 1.6838 (9) | C4—H4B | 0.9700 |
Si1—F1vii | 1.6838 (9) | C2—C3 | 1.345 (3) |
Si1—F1viii | 1.6838 (9) | C2—H2A | 0.9300 |
Si1—F1ix | 1.6838 (9) | C6—C5xii | 1.380 (2) |
Si1—F1x | 1.6838 (9) | C6—H6A | 0.9300 |
N2—C1 | 1.338 (2) | C1—H1A | 0.9300 |
N2—C3 | 1.363 (2) | C3—H3A | 0.9300 |
N1i—Cd1—N1ii | 92.27 (5) | F1ix—Si1—F1x | 180.00 (13) |
N1i—Cd1—N1iii | 87.73 (5) | C1—N2—C3 | 106.54 (15) |
N1ii—Cd1—N1iii | 180.0 | C1—N2—C4 | 124.97 (15) |
N1i—Cd1—N1 | 180.00 (7) | C3—N2—C4 | 128.12 (16) |
N1ii—Cd1—N1 | 87.73 (5) | C6xi—C5—C6 | 119.22 (17) |
N1iii—Cd1—N1 | 92.27 (5) | C6xi—C5—C4 | 120.90 (16) |
N1i—Cd1—N1iv | 92.27 (5) | C6—C5—C4 | 119.81 (15) |
N1ii—Cd1—N1iv | 92.27 (5) | C1—N1—C2 | 104.80 (15) |
N1iii—Cd1—N1iv | 87.73 (5) | C1—N1—Cd1 | 127.37 (12) |
N1—Cd1—N1iv | 87.73 (5) | C2—N1—Cd1 | 127.70 (12) |
N1i—Cd1—N1v | 87.73 (5) | N2—C4—C5 | 110.62 (13) |
N1ii—Cd1—N1v | 87.73 (5) | N2—C4—H4A | 109.5 |
N1iii—Cd1—N1v | 92.27 (5) | C5—C4—H4A | 109.5 |
N1—Cd1—N1v | 92.27 (5) | N2—C4—H4B | 109.5 |
N1iv—Cd1—N1v | 180.00 (6) | C5—C4—H4B | 109.5 |
F1—Si1—F1vi | 180.0 | H4A—C4—H4B | 108.1 |
F1—Si1—F1vii | 89.86 (5) | C3—C2—N1 | 110.01 (17) |
F1vi—Si1—F1vii | 90.14 (5) | C3—C2—H2A | 125.0 |
F1—Si1—F1viii | 90.14 (5) | N1—C2—H2A | 125.0 |
F1vi—Si1—F1viii | 89.86 (5) | C5xii—C6—C5 | 120.77 (17) |
F1vii—Si1—F1viii | 180.00 (8) | C5xii—C6—H6A | 119.6 |
F1—Si1—F1ix | 89.86 (5) | C5—C6—H6A | 119.6 |
F1vi—Si1—F1ix | 90.14 (5) | N1—C1—N2 | 112.07 (16) |
F1vii—Si1—F1ix | 90.14 (5) | N1—C1—H1A | 124.0 |
F1viii—Si1—F1ix | 89.86 (5) | N2—C1—H1A | 124.0 |
F1—Si1—F1x | 90.14 (5) | C2—C3—N2 | 106.58 (17) |
F1vi—Si1—F1x | 89.86 (5) | C2—C3—H3A | 126.7 |
F1vii—Si1—F1x | 89.86 (5) | N2—C3—H3A | 126.7 |
F1viii—Si1—F1x | 90.14 (5) | ||
C1—N2—C4—C5 | −87.9 (2) | C2—N1—C1—N2 | −0.4 (2) |
C3—N2—C4—C5 | 84.1 (2) | Cd1—N1—C1—N2 | −176.52 (11) |
C6xi—C5—C4—N2 | −104.42 (18) | C3—N2—C1—N1 | 0.9 (2) |
C6—C5—C4—N2 | 72.7 (2) | C4—N2—C1—N1 | 174.37 (15) |
C1—N1—C2—C3 | −0.2 (2) | N1—C2—C3—N2 | 0.8 (2) |
Cd1—N1—C2—C3 | 175.85 (14) | C1—N2—C3—C2 | −1.0 (2) |
C6xi—C5—C6—C5xii | 0.8 (3) | C4—N2—C3—C2 | −174.19 (17) |
C4—C5—C6—C5xii | −176.40 (11) |
Symmetry codes: (i) −x+2, −y, −z+1; (ii) y+1, −x+y+1, −z+1; (iii) −y+1, x−y−1, z; (iv) x−y, x−1, −z+1; (v) −x+y+2, −x+1, z; (vi) −x, −y, −z; (vii) y, −x+y, −z; (viii) −y, x−y, z; (ix) x−y, x, −z; (x) −x+y, −x, z; (xi) −y+1, x−y, z; (xii) −x+y+1, −x+1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4B···F1xiii | 0.97 | 2.52 | 3.319 (2) | 139 |
C1—H1A···F1xiv | 0.93 | 2.40 | 3.259 (2) | 153 |
C1—H1A···F1xiii | 0.93 | 2.46 | 3.0247 (19) | 119 |
Symmetry codes: (xiii) x−y+1, x, −z+1; (xiv) −x+1, −y, −z+1. |