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The judicious selection of suitable ligands is vitally important in the construction of novel metal–organic frameworks (MOFs) with fascinating structures and interesting properties. Recently, imidazole-containing multidentate ligands have received much attention. Two new Cd
II coordination frameworks, namely, poly[tris{μ-1,4-bis[(1
H-imidazol-1-yl)methyl]benzene-κ
2N3:
N3′}tetrakis(nitrato-κ
2O,
O′)dicadmium], [Cd
2(NO
3)
4(C
14H
14N
4)
3]
n, (I), and poly[[bis{μ
3-1,3,5-tris[(1
H-imidazol-1-yl)methyl]benzene-κ
3N3:
N3′:
N3′′}cadmium] hexafluorosilicate], {[Cd(C
18H
18N
6)
2](SiF
6)}
n, (II), have been synthesized and characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. In polymer (I), the 1,4-bis[(1
H-imidazol-1-yl)methyl]benzene ligand bridges Cd
2+ ions with a distorted seven-coordinated pentagonal bipyramidal geometry, forming a one-dimensional ladder chain, and the nitrate anions coordinate to the Cd
2+ ions in a terminal bidentate fashion. In the crystal, adjacent chains are further connected by C—H
O hydrogen bonds to generate a two-dimensional (2D) supramolecular structure. Polymer (II) exhibits a 2D layered structure in which 1,3,5-tris[(1
H-imidazol-1-yl)methyl] benzene ligands join Cd
2+ centres having a six-coordinated octahedral structure. The layers are connected by hexafluorosilicate anions
via C—H
F hydrogen-bond interactions, giving rise to a three-dimensional supramolecular network structure in the solid state. In addition, powder X-ray diffraction (PXRD) patterns were recorded, thermogravimetric analyses (TGA) carried out and fluorescence properties investigated.
Supporting information
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).
Poly[tris{µ-1,4-bis[(1
H-imidazol-1-yl)methyl]benzene-
κ2N3:
N3'}tetrakis(nitrato-
κ2O,
O')dicadmium] (I)
top
Crystal data top
[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 |
Data collection top
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 top
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 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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) | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
Hydrogen-bond geometry (Å, º) top
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. |
Poly[[bis{µ
3-1,3,5-tris[(1
H-imidazol-1-yl)methyl]benzene-
κ3N3:
N3':
N3''}cadmium] hexafluorosilicate] (II)
top
Crystal data top
[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 |
Data collection top
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 top
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 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | 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* | |
Atomic displacement parameters (Å2) top | 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) |
Geometric parameters (Å, º) top
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. |
Hydrogen-bond geometry (Å, º) top
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. |
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