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In the structures of the CdII pseudohalide coordination polymer poly[[diaquabis[μ2-3,3′-bis(1,2,4-triazol-4-yl)-1,1′-biadamantane-κ2N1:N1′]cadmium(II)] dithiocyanate dihydrate], {[Cd(C24H32N6)2(H2O)2](NCS)2·2H2O}n, (I), and the isomorphous selenocyanate analogue, {[Cd(C24H32N6)2(H2O)2](NCSe)2·2H2O}n, (II), the CdII cations occupy inversion centres and have octahedral CdN4O2 environments, completed by four N atoms of the organic ligands [Cd—N = 2.316 (2) and 2.361 (2) Å for (I), and 2.313 (3) and 2.372 (3) Å for (II)] and two trans-coordinated aqua ligands [Cd—O = 2.3189 (15) Å for (I) and 2.323 (2) Å for (II)]. In each compound, the ligand displays a bidentate N1:N1′-bridging mode, connecting the metal centres at a distance of 14.66 Å into two-dimensional nets of (4,4)-topology, while the uncoordinated thio(seleno)cyanate anions reside inside the net cavities. Hydrogen bonding between the water molecules, anions and 1,2,4-triazole N atoms supports the tight packing, with an interlayer distance of 6.09 Å.
Supporting information
CCDC references: 786799; 786800
For both compounds, data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-NT (Bruker, 1999); data reduction: SAINT-NT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Version 1.70.01; Farrugia, 1999).
(I) poly[[diaquabis[µ
2-3,3'-bis(1,2,4-triazol-4-yl)-1,1'-biadamantane-
κ2N1:
N1']cadmium(II)] dithiocyanate dihydrate],
top
Crystal data top
[Cd(C24H32N6)2(H2O)2](NCS)2·2H2O | F(000) = 1164 |
Mr = 1109.74 | Dx = 1.454 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 6.8689 (4) Å | Cell parameters from 13522 reflections |
b = 20.3896 (12) Å | θ = 2.0–27.1° |
c = 18.3330 (11) Å | µ = 0.57 mm−1 |
β = 99.242 (2)° | T = 213 K |
V = 2534.3 (3) Å3 | Plate, colourless |
Z = 2 | 0.22 × 0.20 × 0.04 mm |
Data collection top
Bruker APEXII area-detector diffractometer | 5535 independent reflections |
Radiation source: fine-focus sealed tube | 4109 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 27.1°, θmin = 2.0° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 2003) | h = −8→7 |
Tmin = 0.884, Tmax = 0.977 | k = −26→25 |
13522 measured reflections | l = −23→20 |
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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.098 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0415P)2] where P = (Fo2 + 2Fc2)/3 |
5535 reflections | (Δ/σ)max < 0.001 |
322 parameters | Δρmax = 0.59 e Å−3 |
4 restraints | Δρmin = −0.51 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 | |
Cd1 | 0.0000 | 0.5000 | 0.0000 | 0.02593 (10) | |
S1 | 0.68529 (19) | 0.28388 (6) | 0.25383 (7) | 0.0891 (4) | |
O1 | −0.18791 (9) | 0.460010 (18) | 0.08457 (9) | 0.0438 (5) | |
H1W | −0.1309 | 0.4252 | 0.1024 | 0.066* | |
H2W | −0.3055 | 0.4504 | 0.0655 | 0.066* | |
O2 | −0.06224 (6) | 0.34054 (15) | 0.13331 (6) | 0.1004 (11) | |
H3W | −0.1127 | 0.3258 | 0.1694 | 0.151* | |
H4W | 0.0616 | 0.3438 | 0.1470 | 0.151* | |
N1 | 0.2226 (3) | 0.41096 (11) | 0.01136 (13) | 0.0352 (6) | |
N2 | 0.4243 (4) | 0.41353 (11) | 0.02615 (15) | 0.0425 (6) | |
N3 | 0.3364 (3) | 0.31191 (10) | 0.00065 (11) | 0.0269 (5) | |
N4 | 0.7781 (4) | 0.11910 (11) | 0.39708 (13) | 0.0381 (6) | |
N5 | 0.7919 (3) | 0.05173 (11) | 0.40544 (12) | 0.0325 (5) | |
N6 | 0.5522 (3) | 0.07241 (10) | 0.31510 (11) | 0.0267 (5) | |
N7 | 0.3437 (6) | 0.3465 (2) | 0.1897 (2) | 0.0959 (13) | |
C1 | 0.1740 (4) | 0.35045 (13) | −0.00343 (17) | 0.0377 (7) | |
H1 | 0.0436 | 0.3353 | −0.0154 | 0.045* | |
C2 | 0.4856 (4) | 0.35382 (15) | 0.01942 (18) | 0.0411 (8) | |
H2 | 0.6192 | 0.3416 | 0.0269 | 0.049* | |
C3 | 0.6343 (4) | 0.12912 (14) | 0.34300 (15) | 0.0348 (7) | |
H3 | 0.5923 | 0.1709 | 0.3253 | 0.042* | |
C4 | 0.6568 (4) | 0.02526 (14) | 0.35631 (15) | 0.0322 (6) | |
H4 | 0.6350 | −0.0201 | 0.3503 | 0.039* | |
C5 | 0.3414 (4) | 0.23987 (12) | −0.01068 (14) | 0.0252 (6) | |
C6 | 0.5453 (4) | 0.21938 (13) | −0.02605 (15) | 0.0317 (6) | |
H6A | 0.6465 | 0.2315 | 0.0157 | 0.038* | |
H6B | 0.5747 | 0.2417 | −0.0703 | 0.038* | |
C7 | 0.5452 (4) | 0.14468 (13) | −0.03756 (15) | 0.0345 (7) | |
H7 | 0.6768 | 0.1309 | −0.0474 | 0.041* | |
C8 | 0.5035 (4) | 0.11108 (13) | 0.03278 (15) | 0.0287 (6) | |
H8A | 0.6047 | 0.1238 | 0.0743 | 0.034* | |
H8B | 0.5103 | 0.0634 | 0.0268 | 0.034* | |
C9 | 0.2977 (3) | 0.12994 (12) | 0.05023 (13) | 0.0223 (5) | |
C10 | 0.2967 (4) | 0.20543 (12) | 0.05869 (13) | 0.0238 (6) | |
H10A | 0.1671 | 0.2196 | 0.0686 | 0.029* | |
H10B | 0.3954 | 0.2182 | 0.1010 | 0.029* | |
C11 | 0.1855 (4) | 0.22183 (14) | −0.07698 (15) | 0.0366 (7) | |
H11A | 0.2136 | 0.2443 | −0.1214 | 0.044* | |
H11B | 0.0546 | 0.2355 | −0.0680 | 0.044* | |
C12 | 0.1902 (4) | 0.14749 (14) | −0.08790 (15) | 0.0384 (7) | |
H12 | 0.0891 | 0.1352 | −0.1304 | 0.046* | |
C13 | 0.3911 (5) | 0.12645 (15) | −0.10324 (16) | 0.0470 (8) | |
H13A | 0.4203 | 0.1484 | −0.1478 | 0.056* | |
H13B | 0.3926 | 0.0790 | −0.1114 | 0.056* | |
C14 | 0.1452 (4) | 0.11267 (13) | −0.01841 (15) | 0.0335 (7) | |
H14A | 0.1454 | 0.0651 | −0.0263 | 0.040* | |
H14B | 0.0134 | 0.1253 | −0.0096 | 0.040* | |
C15 | 0.3795 (4) | 0.06503 (13) | 0.25504 (14) | 0.0263 (6) | |
C16 | 0.3434 (4) | −0.00767 (13) | 0.23839 (16) | 0.0337 (7) | |
H16A | 0.3158 | −0.0305 | 0.2827 | 0.040* | |
H16B | 0.4608 | −0.0275 | 0.2234 | 0.040* | |
C17 | 0.1673 (5) | −0.01418 (14) | 0.17610 (17) | 0.0407 (8) | |
H17 | 0.1428 | −0.0612 | 0.1648 | 0.049* | |
C18 | −0.0148 (5) | 0.01558 (17) | 0.20049 (19) | 0.0518 (9) | |
H18A | −0.0436 | −0.0071 | 0.2447 | 0.062* | |
H18B | −0.1288 | 0.0105 | 0.1612 | 0.062* | |
C19 | 0.0225 (4) | 0.08832 (16) | 0.21733 (16) | 0.0402 (8) | |
H19 | −0.0962 | 0.1080 | 0.2328 | 0.048* | |
C20 | 0.1982 (4) | 0.09555 (15) | 0.28000 (15) | 0.0363 (7) | |
H20A | 0.2224 | 0.1420 | 0.2917 | 0.044* | |
H20B | 0.1699 | 0.0733 | 0.3245 | 0.044* | |
C21 | 0.4257 (3) | 0.09982 (12) | 0.18581 (13) | 0.0224 (5) | |
H21A | 0.5433 | 0.0801 | 0.1708 | 0.027* | |
H21B | 0.4541 | 0.1461 | 0.1971 | 0.027* | |
C22 | 0.2509 (4) | 0.09455 (12) | 0.12144 (14) | 0.0238 (6) | |
C23 | 0.2095 (4) | 0.02081 (13) | 0.10693 (15) | 0.0338 (7) | |
H23A | 0.0960 | 0.0158 | 0.0675 | 0.041* | |
H23B | 0.3239 | 0.0005 | 0.0903 | 0.041* | |
C24 | 0.0692 (4) | 0.12420 (14) | 0.14924 (15) | 0.0336 (7) | |
H24A | 0.0943 | 0.1706 | 0.1613 | 0.040* | |
H24B | −0.0451 | 0.1217 | 0.1098 | 0.040* | |
C25 | 0.4835 (7) | 0.3201 (2) | 0.2158 (2) | 0.0625 (11) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.02848 (16) | 0.02144 (15) | 0.02618 (16) | 0.00002 (13) | −0.00077 (10) | −0.00286 (12) |
S1 | 0.0970 (9) | 0.0751 (8) | 0.1019 (10) | 0.0054 (7) | 0.0363 (8) | 0.0356 (7) |
O1 | 0.0402 (12) | 0.0502 (13) | 0.0419 (13) | −0.0120 (10) | 0.0092 (10) | 0.0000 (11) |
O2 | 0.074 (2) | 0.121 (3) | 0.110 (3) | 0.0163 (19) | 0.0265 (18) | 0.063 (2) |
N1 | 0.0347 (14) | 0.0241 (12) | 0.0461 (15) | 0.0023 (11) | 0.0040 (11) | −0.0022 (11) |
N2 | 0.0359 (14) | 0.0265 (13) | 0.0670 (18) | −0.0042 (11) | 0.0143 (13) | −0.0091 (13) |
N3 | 0.0253 (12) | 0.0230 (11) | 0.0308 (13) | 0.0001 (10) | −0.0004 (9) | 0.0019 (10) |
N4 | 0.0428 (15) | 0.0306 (13) | 0.0368 (14) | −0.0005 (12) | −0.0056 (11) | 0.0006 (11) |
N5 | 0.0338 (14) | 0.0306 (13) | 0.0307 (13) | 0.0034 (11) | −0.0017 (10) | 0.0053 (11) |
N6 | 0.0304 (13) | 0.0245 (12) | 0.0234 (12) | 0.0017 (10) | −0.0010 (9) | 0.0022 (10) |
N7 | 0.090 (3) | 0.136 (4) | 0.060 (3) | 0.003 (3) | 0.005 (2) | −0.012 (2) |
C1 | 0.0293 (16) | 0.0282 (16) | 0.053 (2) | 0.0036 (13) | −0.0003 (13) | 0.0015 (14) |
C2 | 0.0270 (16) | 0.0342 (17) | 0.062 (2) | −0.0002 (14) | 0.0059 (15) | −0.0106 (15) |
C3 | 0.0416 (17) | 0.0267 (15) | 0.0326 (16) | 0.0020 (13) | −0.0043 (13) | −0.0009 (13) |
C4 | 0.0373 (17) | 0.0277 (14) | 0.0303 (16) | 0.0040 (13) | 0.0014 (12) | 0.0061 (13) |
C5 | 0.0262 (14) | 0.0204 (13) | 0.0269 (14) | 0.0010 (11) | −0.0016 (11) | 0.0003 (11) |
C6 | 0.0331 (15) | 0.0299 (15) | 0.0330 (15) | 0.0046 (13) | 0.0084 (12) | 0.0042 (13) |
C7 | 0.0407 (17) | 0.0295 (16) | 0.0355 (17) | 0.0092 (13) | 0.0129 (13) | −0.0011 (13) |
C8 | 0.0295 (15) | 0.0244 (14) | 0.0326 (15) | 0.0050 (12) | 0.0062 (11) | 0.0008 (13) |
C9 | 0.0225 (13) | 0.0195 (13) | 0.0230 (13) | 0.0010 (11) | −0.0023 (10) | 0.0003 (11) |
C10 | 0.0187 (13) | 0.0247 (14) | 0.0267 (14) | 0.0027 (11) | 0.0000 (10) | −0.0016 (11) |
C11 | 0.0395 (17) | 0.0346 (16) | 0.0315 (16) | 0.0005 (14) | −0.0067 (12) | 0.0035 (13) |
C12 | 0.0528 (19) | 0.0311 (16) | 0.0256 (16) | −0.0076 (15) | −0.0109 (13) | −0.0022 (13) |
C13 | 0.077 (2) | 0.0357 (18) | 0.0300 (17) | 0.0039 (17) | 0.0125 (16) | −0.0040 (14) |
C14 | 0.0350 (16) | 0.0270 (15) | 0.0343 (16) | −0.0034 (13) | −0.0078 (12) | −0.0028 (13) |
C15 | 0.0247 (14) | 0.0291 (14) | 0.0240 (14) | −0.0009 (12) | 0.0005 (10) | 0.0011 (12) |
C16 | 0.0396 (16) | 0.0281 (16) | 0.0319 (15) | −0.0063 (13) | 0.0010 (12) | 0.0068 (12) |
C17 | 0.0439 (18) | 0.0297 (17) | 0.0455 (19) | −0.0182 (13) | −0.0021 (14) | 0.0016 (13) |
C18 | 0.0366 (18) | 0.069 (2) | 0.049 (2) | −0.0233 (17) | 0.0035 (15) | 0.0116 (17) |
C19 | 0.0214 (15) | 0.058 (2) | 0.0418 (18) | −0.0006 (14) | 0.0086 (13) | 0.0046 (16) |
C20 | 0.0364 (17) | 0.0434 (18) | 0.0307 (16) | 0.0012 (14) | 0.0101 (13) | 0.0025 (14) |
C21 | 0.0225 (13) | 0.0202 (13) | 0.0236 (14) | 0.0007 (10) | 0.0011 (10) | −0.0007 (11) |
C22 | 0.0204 (13) | 0.0222 (13) | 0.0276 (14) | −0.0020 (11) | 0.0005 (10) | 0.0001 (11) |
C23 | 0.0369 (17) | 0.0284 (14) | 0.0328 (16) | −0.0080 (13) | −0.0040 (12) | 0.0004 (13) |
C24 | 0.0219 (14) | 0.0452 (18) | 0.0328 (16) | 0.0065 (13) | 0.0017 (11) | 0.0049 (13) |
C25 | 0.080 (3) | 0.068 (3) | 0.041 (2) | −0.014 (2) | 0.016 (2) | −0.0155 (19) |
Geometric parameters (Å, º) top
Cd1—N5i | 2.316 (2) | C9—C10 | 1.547 (3) |
Cd1—N5ii | 2.316 (2) | C9—C22 | 1.569 (3) |
Cd1—O1iii | 2.3189 (15) | C10—H10A | 0.9800 |
Cd1—O1 | 2.3189 (15) | C10—H10B | 0.9800 |
Cd1—N1iii | 2.361 (2) | C11—C12 | 1.530 (4) |
Cd1—N1 | 2.361 (2) | C11—H11A | 0.9800 |
S1—C25 | 1.626 (5) | C11—H11B | 0.9800 |
O1—H1W | 0.8500 | C12—C13 | 1.514 (4) |
O1—H2W | 0.8500 | C12—C14 | 1.533 (4) |
O2—H3W | 0.8500 | C12—H12 | 0.9900 |
O2—H4W | 0.8500 | C13—H13A | 0.9800 |
N1—C1 | 1.295 (3) | C13—H13B | 0.9800 |
N1—N2 | 1.369 (3) | C14—H14A | 0.9800 |
N2—C2 | 1.301 (3) | C14—H14B | 0.9800 |
N3—C2 | 1.336 (3) | C15—C16 | 1.526 (3) |
N3—C1 | 1.356 (3) | C15—C20 | 1.527 (4) |
N3—C5 | 1.485 (3) | C15—C21 | 1.531 (3) |
N4—C3 | 1.298 (3) | C16—C17 | 1.530 (4) |
N4—N5 | 1.384 (3) | C16—H16A | 0.9800 |
N5—C4 | 1.302 (3) | C16—H16B | 0.9800 |
N6—C3 | 1.351 (3) | C17—C18 | 1.521 (5) |
N6—C4 | 1.356 (3) | C17—C23 | 1.523 (4) |
N6—C15 | 1.491 (3) | C17—H17 | 0.9900 |
N7—C25 | 1.137 (5) | C18—C19 | 1.528 (4) |
C1—H1 | 0.9400 | C18—H18A | 0.9800 |
C2—H2 | 0.9400 | C18—H18B | 0.9800 |
C3—H3 | 0.9400 | C19—C24 | 1.525 (4) |
C4—H4 | 0.9400 | C19—C20 | 1.534 (4) |
C5—C10 | 1.527 (3) | C19—H19 | 0.9900 |
C5—C11 | 1.530 (4) | C20—H20A | 0.9800 |
C5—C6 | 1.530 (4) | C20—H20B | 0.9800 |
C6—C7 | 1.538 (4) | C21—C22 | 1.547 (3) |
C6—H6A | 0.9800 | C21—H21A | 0.9800 |
C6—H6B | 0.9800 | C21—H21B | 0.9800 |
C7—C13 | 1.516 (4) | C22—C24 | 1.545 (3) |
C7—C8 | 1.527 (4) | C22—C23 | 1.545 (3) |
C7—H7 | 0.9900 | C23—H23A | 0.9800 |
C8—C9 | 1.547 (3) | C23—H23B | 0.9800 |
C8—H8A | 0.9800 | C24—H24A | 0.9800 |
C8—H8B | 0.9800 | C24—H24B | 0.9800 |
C9—C14 | 1.543 (3) | | |
| | | |
N5i—Cd1—N5ii | 180.0 | C12—C11—H11A | 110.0 |
N5i—Cd1—O1iii | 89.85 (6) | C5—C11—H11B | 110.0 |
N5ii—Cd1—O1iii | 90.15 (6) | C12—C11—H11B | 110.0 |
N5i—Cd1—O1 | 90.15 (6) | H11A—C11—H11B | 108.4 |
N5ii—Cd1—O1 | 89.85 (6) | C13—C12—C11 | 110.1 (2) |
O1iii—Cd1—O1 | 180.0 | C13—C12—C14 | 109.6 (2) |
N5i—Cd1—N1iii | 91.66 (8) | C11—C12—C14 | 109.8 (2) |
N5ii—Cd1—N1iii | 88.34 (8) | C13—C12—H12 | 109.1 |
O1iii—Cd1—N1iii | 95.32 (6) | C11—C12—H12 | 109.1 |
O1—Cd1—N1iii | 84.68 (6) | C14—C12—H12 | 109.1 |
N5i—Cd1—N1 | 88.34 (8) | C12—C13—C7 | 108.9 (2) |
N5ii—Cd1—N1 | 91.66 (8) | C12—C13—H13A | 109.9 |
O1iii—Cd1—N1 | 84.68 (6) | C7—C13—H13A | 109.9 |
O1—Cd1—N1 | 95.32 (6) | C12—C13—H13B | 109.9 |
N1iii—Cd1—N1 | 180.0 | C7—C13—H13B | 109.9 |
Cd1—O1—H1W | 106.2 | H13A—C13—H13B | 108.3 |
Cd1—O1—H2W | 113.6 | C12—C14—C9 | 111.8 (2) |
H1W—O1—H2W | 108.4 | C12—C14—H14A | 109.3 |
H3W—O2—H4W | 108.2 | C9—C14—H14A | 109.3 |
C1—N1—N2 | 107.2 (2) | C12—C14—H14B | 109.3 |
C1—N1—Cd1 | 124.9 (2) | C9—C14—H14B | 109.3 |
N2—N1—Cd1 | 127.47 (17) | H14A—C14—H14B | 107.9 |
C2—N2—N1 | 106.1 (2) | N6—C15—C16 | 109.3 (2) |
C2—N3—C1 | 103.5 (2) | N6—C15—C20 | 109.1 (2) |
C2—N3—C5 | 129.4 (2) | C16—C15—C20 | 110.0 (2) |
C1—N3—C5 | 127.1 (2) | N6—C15—C21 | 108.6 (2) |
C3—N4—N5 | 105.7 (2) | C16—C15—C21 | 109.5 (2) |
C4—N5—N4 | 107.9 (2) | C20—C15—C21 | 110.3 (2) |
C4—N5—Cd1iv | 127.91 (19) | C15—C16—C17 | 108.5 (2) |
N4—N5—Cd1iv | 123.92 (17) | C15—C16—H16A | 110.0 |
C3—N6—C4 | 104.1 (2) | C17—C16—H16A | 110.0 |
C3—N6—C15 | 126.9 (2) | C15—C16—H16B | 110.0 |
C4—N6—C15 | 128.9 (2) | C17—C16—H16B | 110.0 |
N1—C1—N3 | 111.0 (3) | H16A—C16—H16B | 108.4 |
N1—C1—H1 | 124.5 | C18—C17—C23 | 109.5 (3) |
N3—C1—H1 | 124.5 | C18—C17—C16 | 109.6 (3) |
N2—C2—N3 | 112.1 (3) | C23—C17—C16 | 110.3 (2) |
N2—C2—H2 | 123.9 | C18—C17—H17 | 109.1 |
N3—C2—H2 | 123.9 | C23—C17—H17 | 109.1 |
N4—C3—N6 | 112.0 (3) | C16—C17—H17 | 109.1 |
N4—C3—H3 | 124.0 | C17—C18—C19 | 109.1 (2) |
N6—C3—H3 | 124.0 | C17—C18—H18A | 109.9 |
N5—C4—N6 | 110.3 (3) | C19—C18—H18A | 109.9 |
N5—C4—H4 | 124.9 | C17—C18—H18B | 109.9 |
N6—C4—H4 | 124.9 | C19—C18—H18B | 109.9 |
N3—C5—C10 | 109.0 (2) | H18A—C18—H18B | 108.3 |
N3—C5—C11 | 108.6 (2) | C24—C19—C18 | 110.5 (3) |
C10—C5—C11 | 110.0 (2) | C24—C19—C20 | 108.9 (2) |
N3—C5—C6 | 109.8 (2) | C18—C19—C20 | 109.3 (3) |
C10—C5—C6 | 109.9 (2) | C24—C19—H19 | 109.4 |
C11—C5—C6 | 109.4 (2) | C18—C19—H19 | 109.4 |
C5—C6—C7 | 108.4 (2) | C20—C19—H19 | 109.4 |
C5—C6—H6A | 110.0 | C15—C20—C19 | 108.5 (2) |
C7—C6—H6A | 110.0 | C15—C20—H20A | 110.0 |
C5—C6—H6B | 110.0 | C19—C20—H20A | 110.0 |
C7—C6—H6B | 110.0 | C15—C20—H20B | 110.0 |
H6A—C6—H6B | 108.4 | C19—C20—H20B | 110.0 |
C13—C7—C8 | 111.0 (2) | H20A—C20—H20B | 108.4 |
C13—C7—C6 | 109.7 (2) | C15—C21—C22 | 111.2 (2) |
C8—C7—C6 | 108.9 (2) | C15—C21—H21A | 109.4 |
C13—C7—H7 | 109.1 | C22—C21—H21A | 109.4 |
C8—C7—H7 | 109.1 | C15—C21—H21B | 109.4 |
C6—C7—H7 | 109.1 | C22—C21—H21B | 109.4 |
C7—C8—C9 | 111.4 (2) | H21A—C21—H21B | 108.0 |
C7—C8—H8A | 109.3 | C24—C22—C23 | 107.6 (2) |
C9—C8—H8A | 109.3 | C24—C22—C21 | 106.9 (2) |
C7—C8—H8B | 109.3 | C23—C22—C21 | 107.3 (2) |
C9—C8—H8B | 109.3 | C24—C22—C9 | 112.3 (2) |
H8A—C8—H8B | 108.0 | C23—C22—C9 | 111.2 (2) |
C14—C9—C10 | 107.2 (2) | C21—C22—C9 | 111.41 (19) |
C14—C9—C8 | 107.3 (2) | C17—C23—C22 | 111.5 (2) |
C10—C9—C8 | 106.7 (2) | C17—C23—H23A | 109.3 |
C14—C9—C22 | 111.7 (2) | C22—C23—H23A | 109.3 |
C10—C9—C22 | 111.7 (2) | C17—C23—H23B | 109.3 |
C8—C9—C22 | 112.0 (2) | C22—C23—H23B | 109.3 |
C5—C10—C9 | 111.7 (2) | H23A—C23—H23B | 108.0 |
C5—C10—H10A | 109.3 | C19—C24—C22 | 111.7 (2) |
C9—C10—H10A | 109.3 | C19—C24—H24A | 109.3 |
C5—C10—H10B | 109.3 | C22—C24—H24A | 109.3 |
C9—C10—H10B | 109.3 | C19—C24—H24B | 109.3 |
H10A—C10—H10B | 107.9 | C22—C24—H24B | 109.3 |
C5—C11—C12 | 108.4 (2) | H24A—C24—H24B | 107.9 |
C5—C11—H11A | 110.0 | N7—C25—S1 | 178.7 (4) |
| | | |
N5i—Cd1—N1—C1 | 150.6 (2) | C14—C12—C13—C7 | −59.9 (3) |
N5ii—Cd1—N1—C1 | −29.4 (2) | C8—C7—C13—C12 | 59.6 (3) |
O1iii—Cd1—N1—C1 | −119.4 (2) | C6—C7—C13—C12 | −60.8 (3) |
O1—Cd1—N1—C1 | 60.6 (2) | C13—C12—C14—C9 | 60.8 (3) |
N5i—Cd1—N1—N2 | −37.3 (2) | C11—C12—C14—C9 | −60.3 (3) |
N5ii—Cd1—N1—N2 | 142.7 (2) | C10—C9—C14—C12 | 57.1 (3) |
O1iii—Cd1—N1—N2 | 52.7 (2) | C8—C9—C14—C12 | −57.2 (3) |
O1—Cd1—N1—N2 | −127.3 (2) | C22—C9—C14—C12 | 179.7 (2) |
C1—N1—N2—C2 | −0.1 (3) | C3—N6—C15—C16 | 177.1 (2) |
Cd1—N1—N2—C2 | −173.3 (2) | C4—N6—C15—C16 | −6.1 (4) |
C3—N4—N5—C4 | 0.0 (3) | C3—N6—C15—C20 | −62.6 (3) |
C3—N4—N5—Cd1iv | −173.95 (18) | C4—N6—C15—C20 | 114.2 (3) |
N2—N1—C1—N3 | −0.2 (3) | C3—N6—C15—C21 | 57.8 (3) |
Cd1—N1—C1—N3 | 173.26 (17) | C4—N6—C15—C21 | −125.5 (3) |
C2—N3—C1—N1 | 0.4 (3) | N6—C15—C16—C17 | −179.4 (2) |
C5—N3—C1—N1 | 178.4 (2) | C20—C15—C16—C17 | 60.8 (3) |
N1—N2—C2—N3 | 0.3 (3) | C21—C15—C16—C17 | −60.5 (3) |
C1—N3—C2—N2 | −0.4 (3) | C15—C16—C17—C18 | −60.7 (3) |
C5—N3—C2—N2 | −178.3 (2) | C15—C16—C17—C23 | 59.9 (3) |
N5—N4—C3—N6 | 0.0 (3) | C23—C17—C18—C19 | −60.1 (3) |
C4—N6—C3—N4 | 0.0 (3) | C16—C17—C18—C19 | 61.0 (3) |
C15—N6—C3—N4 | 177.3 (2) | C17—C18—C19—C24 | 59.0 (3) |
N4—N5—C4—N6 | −0.1 (3) | C17—C18—C19—C20 | −60.8 (3) |
Cd1iv—N5—C4—N6 | 173.61 (16) | N6—C15—C20—C19 | 179.3 (2) |
C3—N6—C4—N5 | 0.1 (3) | C16—C15—C20—C19 | −60.8 (3) |
C15—N6—C4—N5 | −177.3 (2) | C21—C15—C20—C19 | 60.0 (3) |
C2—N3—C5—C10 | 99.6 (3) | C24—C19—C20—C15 | −60.5 (3) |
C1—N3—C5—C10 | −77.9 (3) | C18—C19—C20—C15 | 60.3 (3) |
C2—N3—C5—C11 | −140.5 (3) | N6—C15—C21—C22 | −179.42 (19) |
C1—N3—C5—C11 | 42.0 (3) | C16—C15—C21—C22 | 61.3 (3) |
C2—N3—C5—C6 | −20.9 (4) | C20—C15—C21—C22 | −59.8 (3) |
C1—N3—C5—C6 | 161.6 (3) | C15—C21—C22—C24 | 57.2 (3) |
N3—C5—C6—C7 | −179.9 (2) | C15—C21—C22—C23 | −57.9 (3) |
C10—C5—C6—C7 | 60.1 (3) | C15—C21—C22—C9 | −179.8 (2) |
C11—C5—C6—C7 | −60.8 (3) | C14—C9—C22—C24 | −72.4 (3) |
C5—C6—C7—C13 | 60.8 (3) | C10—C9—C22—C24 | 47.7 (3) |
C5—C6—C7—C8 | −60.9 (3) | C8—C9—C22—C24 | 167.2 (2) |
C13—C7—C8—C9 | −58.8 (3) | C14—C9—C22—C23 | 48.1 (3) |
C6—C7—C8—C9 | 62.0 (3) | C10—C9—C22—C23 | 168.2 (2) |
C7—C8—C9—C14 | 55.8 (3) | C8—C9—C22—C23 | −72.3 (3) |
C7—C8—C9—C10 | −58.8 (3) | C14—C9—C22—C21 | 167.8 (2) |
C7—C8—C9—C22 | 178.7 (2) | C10—C9—C22—C21 | −72.2 (2) |
N3—C5—C10—C9 | 179.46 (19) | C8—C9—C22—C21 | 47.4 (3) |
C11—C5—C10—C9 | 60.4 (3) | C18—C17—C23—C22 | 61.1 (3) |
C6—C5—C10—C9 | −60.1 (3) | C16—C17—C23—C22 | −59.6 (3) |
C14—C9—C10—C5 | −57.1 (3) | C24—C22—C23—C17 | −57.7 (3) |
C8—C9—C10—C5 | 57.6 (3) | C21—C22—C23—C17 | 57.0 (3) |
C22—C9—C10—C5 | −179.8 (2) | C9—C22—C23—C17 | 179.0 (2) |
N3—C5—C11—C12 | −179.5 (2) | C18—C19—C24—C22 | −58.2 (3) |
C10—C5—C11—C12 | −60.2 (3) | C20—C19—C24—C22 | 61.9 (3) |
C6—C5—C11—C12 | 60.6 (3) | C23—C22—C24—C19 | 56.1 (3) |
C5—C11—C12—C13 | −60.8 (3) | C21—C22—C24—C19 | −58.9 (3) |
C5—C11—C12—C14 | 60.0 (3) | C9—C22—C24—C19 | 178.6 (2) |
C11—C12—C13—C7 | 60.9 (3) | | |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) x−1, −y+1/2, z−1/2; (iii) −x, −y+1, −z; (iv) −x+1, y−1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1W···O2 | 0.85 | 1.85 | 2.689 (2) | 167 |
O1—H2W···N2v | 0.85 | 2.02 | 2.868 (2) | 171 |
O2—H3W···S1v | 0.85 | 2.40 | 3.2334 (11) | 169 |
O2—H4W···N7 | 0.85 | 1.97 | 2.817 (4) | 173 |
C1—H1···N4ii | 0.94 | 2.41 | 3.085 (4) | 128 |
C2—H2···O2vi | 0.94 | 2.69 | 3.464 (3) | 140 |
C3—H3···S1 | 0.94 | 2.78 | 3.597 (3) | 146 |
Symmetry codes: (ii) x−1, −y+1/2, z−1/2; (v) x−1, y, z; (vi) x+1, y, z. |
(II) poly[[diaquabis[µ
2-3,3'-bis(1,2,4-triazol-4-yl)-1,1'-biadamantane-
κ2N1:
N1']cadmium(II)] diselenocyanate dihydrate],
top
Crystal data top
[Cd(C24H32N6)2(H2O)2](NCSe)2·2H2O | F(000) = 1236 |
Mr = 1203.54 | Dx = 1.558 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 6.9147 (5) Å | Cell parameters from 13671 reflections |
b = 20.4704 (14) Å | θ = 1.5–26.5° |
c = 18.4190 (15) Å | µ = 1.90 mm−1 |
β = 100.168 (2)° | T = 213 K |
V = 2566.2 (3) Å3 | Plate, colourless |
Z = 2 | 0.21 × 0.12 × 0.09 mm |
Data collection top
Bruker APEXII area-detector diffractometer | 5235 independent reflections |
Radiation source: fine-focus sealed tube | 3469 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.050 |
ω scans | θmax = 26.5°, θmin = 1.5° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 2003) | h = −7→8 |
Tmin = 0.012, Tmax = 0.847 | k = −24→17 |
13671 measured reflections | l = −23→21 |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0553P)2] where P = (Fo2 + 2Fc2)/3 |
5235 reflections | (Δ/σ)max < 0.001 |
322 parameters | Δρmax = 0.89 e Å−3 |
4 restraints | Δρmin = −0.97 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 | |
Cd1 | 0.0000 | 0.5000 | 0.0000 | 0.02848 (15) | |
Se1 | 0.70827 (11) | 0.28331 (4) | 0.25839 (4) | 0.0873 (3) | |
O1 | −0.18602 (11) | 0.46130 (4) | 0.08426 (15) | 0.0504 (9) | |
H1W | −0.1384 | 0.4254 | 0.1026 | 0.076* | |
H2W | −0.3071 | 0.4556 | 0.0669 | 0.076* | |
O2 | −0.05887 (19) | 0.3405 (2) | 0.12867 (6) | 0.1057 (17) | |
H3W | −0.1108 | 0.3239 | 0.1629 | 0.159* | |
H4W | 0.0599 | 0.3500 | 0.1461 | 0.159* | |
N1 | 0.2212 (5) | 0.41051 (17) | 0.0109 (2) | 0.0365 (9) | |
N2 | 0.4212 (5) | 0.41342 (17) | 0.0257 (2) | 0.0430 (10) | |
N3 | 0.3354 (5) | 0.31207 (16) | 0.00089 (19) | 0.0295 (8) | |
N4 | 0.7727 (5) | 0.11757 (17) | 0.3983 (2) | 0.0403 (10) | |
N5 | 0.7880 (5) | 0.05069 (17) | 0.4056 (2) | 0.0358 (9) | |
N6 | 0.5454 (5) | 0.07149 (15) | 0.31581 (18) | 0.0282 (8) | |
N7 | 0.3447 (9) | 0.3492 (3) | 0.1888 (3) | 0.0944 (19) | |
C1 | 0.1752 (7) | 0.3497 (2) | −0.0039 (3) | 0.0404 (12) | |
H1 | 0.0457 | 0.3342 | −0.0165 | 0.048* | |
C2 | 0.4847 (6) | 0.3543 (2) | 0.0200 (3) | 0.0449 (13) | |
H2 | 0.6182 | 0.3426 | 0.0281 | 0.054* | |
C3 | 0.6276 (6) | 0.1277 (2) | 0.3447 (2) | 0.0363 (11) | |
H3 | 0.5844 | 0.1695 | 0.3278 | 0.044* | |
C4 | 0.6508 (6) | 0.0248 (2) | 0.3557 (2) | 0.0326 (10) | |
H4 | 0.6293 | −0.0203 | 0.3489 | 0.039* | |
C5 | 0.3420 (6) | 0.24047 (19) | −0.0102 (2) | 0.0278 (10) | |
C6 | 0.5460 (6) | 0.2198 (2) | −0.0222 (3) | 0.0369 (11) | |
H6A | 0.6442 | 0.2319 | 0.0208 | 0.044* | |
H6B | 0.5786 | 0.2422 | −0.0655 | 0.044* | |
C7 | 0.5487 (6) | 0.1460 (2) | −0.0337 (2) | 0.0356 (11) | |
H7 | 0.6809 | 0.1326 | −0.0417 | 0.043* | |
C8 | 0.5027 (6) | 0.1118 (2) | 0.0359 (3) | 0.0331 (10) | |
H8A | 0.6019 | 0.1240 | 0.0785 | 0.040* | |
H8B | 0.5090 | 0.0643 | 0.0296 | 0.040* | |
C9 | 0.2967 (5) | 0.13085 (18) | 0.0503 (2) | 0.0223 (9) | |
C10 | 0.2941 (5) | 0.20540 (18) | 0.0588 (2) | 0.0253 (9) | |
H10A | 0.3906 | 0.2182 | 0.1020 | 0.030* | |
H10B | 0.1641 | 0.2192 | 0.0671 | 0.030* | |
C11 | 0.1903 (7) | 0.22182 (19) | −0.0773 (2) | 0.0366 (11) | |
H11A | 0.2199 | 0.2440 | −0.1213 | 0.044* | |
H11B | 0.0591 | 0.2354 | −0.0701 | 0.044* | |
C12 | 0.1954 (7) | 0.1478 (2) | −0.0878 (2) | 0.0423 (12) | |
H12 | 0.0958 | 0.1355 | −0.1311 | 0.051* | |
C13 | 0.3965 (7) | 0.1270 (2) | −0.1012 (2) | 0.0450 (12) | |
H13A | 0.4265 | 0.1487 | −0.1453 | 0.054* | |
H13B | 0.3990 | 0.0797 | −0.1090 | 0.054* | |
C14 | 0.1479 (6) | 0.1132 (2) | −0.0195 (2) | 0.0336 (11) | |
H14A | 0.1491 | 0.0659 | −0.0272 | 0.040* | |
H14B | 0.0156 | 0.1257 | −0.0124 | 0.040* | |
C15 | 0.3729 (6) | 0.06486 (19) | 0.2546 (2) | 0.0293 (10) | |
C16 | 0.3345 (7) | −0.0073 (2) | 0.2376 (2) | 0.0362 (11) | |
H16A | 0.3059 | −0.0299 | 0.2814 | 0.043* | |
H16B | 0.4505 | −0.0275 | 0.2233 | 0.043* | |
C17 | 0.1592 (7) | −0.0124 (2) | 0.1747 (3) | 0.0419 (12) | |
H17 | 0.1323 | −0.0591 | 0.1630 | 0.050* | |
C18 | −0.0212 (7) | 0.0181 (3) | 0.1972 (3) | 0.0544 (15) | |
H18A | −0.1342 | 0.0136 | 0.1571 | 0.065* | |
H18B | −0.0518 | −0.0042 | 0.2409 | 0.065* | |
C19 | 0.0185 (6) | 0.0896 (2) | 0.2141 (3) | 0.0425 (12) | |
H19 | −0.0994 | 0.1096 | 0.2286 | 0.051* | |
C20 | 0.1923 (6) | 0.0958 (2) | 0.2784 (2) | 0.0355 (11) | |
H20A | 0.2178 | 0.1420 | 0.2907 | 0.043* | |
H20B | 0.1622 | 0.0734 | 0.3220 | 0.043* | |
C21 | 0.4200 (5) | 0.09979 (18) | 0.1865 (2) | 0.0235 (9) | |
H21A | 0.5371 | 0.0801 | 0.1724 | 0.028* | |
H21B | 0.4489 | 0.1458 | 0.1983 | 0.028* | |
C22 | 0.2473 (5) | 0.09532 (18) | 0.1211 (2) | 0.0239 (9) | |
C23 | 0.2025 (6) | 0.0226 (2) | 0.1052 (2) | 0.0356 (11) | |
H23A | 0.3152 | 0.0018 | 0.0889 | 0.043* | |
H23B | 0.0887 | 0.0185 | 0.0654 | 0.043* | |
C24 | 0.0662 (6) | 0.1255 (2) | 0.1469 (2) | 0.0340 (11) | |
H24A | 0.0919 | 0.1716 | 0.1592 | 0.041* | |
H24B | −0.0471 | 0.1232 | 0.1066 | 0.041* | |
C25 | 0.4906 (10) | 0.3220 (3) | 0.2162 (3) | 0.0659 (17) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0304 (2) | 0.0247 (2) | 0.0277 (2) | −0.0010 (2) | −0.00212 (17) | −0.0035 (2) |
Se1 | 0.0882 (5) | 0.0802 (5) | 0.0974 (6) | 0.0005 (4) | 0.0271 (4) | 0.0294 (4) |
O1 | 0.044 (2) | 0.063 (2) | 0.045 (2) | −0.0154 (17) | 0.0078 (16) | −0.0020 (17) |
O2 | 0.071 (3) | 0.135 (4) | 0.116 (4) | 0.022 (3) | 0.030 (3) | 0.061 (3) |
N1 | 0.033 (2) | 0.030 (2) | 0.045 (2) | 0.0040 (17) | 0.0011 (18) | −0.0012 (17) |
N2 | 0.038 (2) | 0.028 (2) | 0.063 (3) | −0.0056 (18) | 0.010 (2) | −0.0077 (19) |
N3 | 0.0263 (19) | 0.0259 (19) | 0.034 (2) | 0.0007 (16) | −0.0004 (16) | 0.0040 (16) |
N4 | 0.046 (2) | 0.035 (2) | 0.034 (2) | −0.0011 (18) | −0.0087 (19) | 0.0007 (17) |
N5 | 0.042 (2) | 0.032 (2) | 0.032 (2) | 0.0034 (17) | −0.0002 (18) | 0.0030 (17) |
N6 | 0.0326 (19) | 0.0255 (19) | 0.0237 (19) | −0.0004 (15) | −0.0030 (16) | 0.0024 (15) |
N7 | 0.092 (4) | 0.126 (5) | 0.060 (4) | −0.005 (4) | −0.001 (3) | −0.009 (3) |
C1 | 0.034 (3) | 0.031 (3) | 0.052 (3) | 0.002 (2) | −0.003 (2) | 0.006 (2) |
C2 | 0.028 (2) | 0.039 (3) | 0.070 (4) | −0.005 (2) | 0.014 (3) | −0.012 (2) |
C3 | 0.046 (3) | 0.025 (2) | 0.033 (3) | 0.002 (2) | −0.005 (2) | −0.002 (2) |
C4 | 0.041 (3) | 0.024 (2) | 0.030 (3) | 0.003 (2) | 0.001 (2) | 0.0010 (19) |
C5 | 0.030 (2) | 0.023 (2) | 0.029 (2) | 0.0031 (18) | 0.0006 (19) | 0.0015 (18) |
C6 | 0.037 (3) | 0.035 (3) | 0.040 (3) | 0.002 (2) | 0.012 (2) | 0.007 (2) |
C7 | 0.037 (3) | 0.035 (3) | 0.038 (3) | 0.007 (2) | 0.014 (2) | 0.001 (2) |
C8 | 0.031 (2) | 0.027 (2) | 0.041 (3) | 0.0058 (18) | 0.004 (2) | 0.002 (2) |
C9 | 0.0171 (19) | 0.022 (2) | 0.026 (2) | 0.0028 (16) | −0.0007 (17) | −0.0002 (17) |
C10 | 0.020 (2) | 0.024 (2) | 0.030 (2) | 0.0002 (17) | −0.0018 (18) | 0.0006 (18) |
C11 | 0.044 (3) | 0.034 (3) | 0.029 (3) | 0.002 (2) | −0.004 (2) | 0.009 (2) |
C12 | 0.056 (3) | 0.033 (3) | 0.030 (3) | −0.007 (2) | −0.014 (2) | −0.001 (2) |
C13 | 0.073 (4) | 0.035 (3) | 0.029 (3) | −0.004 (2) | 0.015 (3) | −0.005 (2) |
C14 | 0.033 (2) | 0.031 (2) | 0.032 (3) | −0.0019 (19) | −0.007 (2) | −0.0015 (19) |
C15 | 0.030 (2) | 0.029 (2) | 0.026 (2) | −0.0020 (18) | −0.0053 (19) | 0.0024 (18) |
C16 | 0.044 (3) | 0.032 (3) | 0.030 (2) | −0.007 (2) | −0.002 (2) | 0.004 (2) |
C17 | 0.049 (3) | 0.031 (3) | 0.041 (3) | −0.017 (2) | −0.003 (2) | 0.003 (2) |
C18 | 0.038 (3) | 0.077 (4) | 0.046 (3) | −0.026 (3) | 0.001 (2) | 0.013 (3) |
C19 | 0.023 (2) | 0.061 (3) | 0.046 (3) | −0.001 (2) | 0.011 (2) | 0.002 (2) |
C20 | 0.032 (2) | 0.044 (3) | 0.032 (3) | 0.000 (2) | 0.010 (2) | 0.003 (2) |
C21 | 0.022 (2) | 0.021 (2) | 0.027 (2) | 0.0008 (16) | 0.0002 (18) | 0.0013 (17) |
C22 | 0.023 (2) | 0.023 (2) | 0.024 (2) | 0.0001 (17) | −0.0013 (18) | 0.0015 (17) |
C23 | 0.036 (2) | 0.032 (2) | 0.036 (3) | −0.009 (2) | −0.003 (2) | 0.0000 (19) |
C24 | 0.020 (2) | 0.047 (3) | 0.034 (3) | 0.0033 (19) | 0.0015 (19) | 0.004 (2) |
C25 | 0.078 (4) | 0.081 (5) | 0.039 (3) | −0.014 (3) | 0.010 (3) | −0.023 (3) |
Geometric parameters (Å, º) top
Cd1—N5i | 2.313 (3) | C9—C14 | 1.541 (5) |
Cd1—N5ii | 2.313 (3) | C9—C22 | 1.582 (5) |
Cd1—O1 | 2.323 (2) | C10—H10A | 0.9800 |
Cd1—O1iii | 2.323 (2) | C10—H10B | 0.9800 |
Cd1—N1iii | 2.372 (3) | C11—C12 | 1.528 (6) |
Cd1—N1 | 2.372 (3) | C11—H11A | 0.9800 |
Se1—C25 | 1.756 (7) | C11—H11B | 0.9800 |
O1—H1W | 0.8500 | C12—C13 | 1.515 (6) |
O1—H2W | 0.8500 | C12—C14 | 1.530 (6) |
O2—H3W | 0.8500 | C12—H12 | 0.9900 |
O2—H4W | 0.8500 | C13—H13A | 0.9800 |
N1—C1 | 1.301 (5) | C13—H13B | 0.9800 |
N1—N2 | 1.363 (5) | C14—H14A | 0.9800 |
N2—C2 | 1.297 (6) | C14—H14B | 0.9800 |
N3—C1 | 1.340 (5) | C15—C16 | 1.523 (5) |
N3—C2 | 1.345 (5) | C15—C21 | 1.529 (5) |
N3—C5 | 1.482 (5) | C15—C20 | 1.531 (6) |
N4—C3 | 1.295 (5) | C16—C17 | 1.526 (6) |
N4—N5 | 1.378 (5) | C16—H16A | 0.9800 |
N5—C4 | 1.310 (5) | C16—H16B | 0.9800 |
N6—C4 | 1.341 (5) | C17—C18 | 1.517 (7) |
N6—C3 | 1.351 (5) | C17—C23 | 1.541 (6) |
N6—C15 | 1.496 (5) | C17—H17 | 0.9900 |
N7—C25 | 1.185 (7) | C18—C19 | 1.510 (7) |
C1—H1 | 0.9400 | C18—H18A | 0.9800 |
C2—H2 | 0.9400 | C18—H18B | 0.9800 |
C3—H3 | 0.9400 | C19—C24 | 1.525 (6) |
C4—H4 | 0.9400 | C19—C20 | 1.536 (6) |
C5—C11 | 1.522 (5) | C19—H19 | 0.9900 |
C5—C6 | 1.526 (6) | C20—H20A | 0.9800 |
C5—C10 | 1.545 (5) | C20—H20B | 0.9800 |
C6—C7 | 1.527 (6) | C21—C22 | 1.541 (5) |
C6—H6A | 0.9800 | C21—H21A | 0.9800 |
C6—H6B | 0.9800 | C21—H21B | 0.9800 |
C7—C13 | 1.531 (6) | C22—C23 | 1.538 (5) |
C7—C8 | 1.542 (6) | C22—C24 | 1.544 (5) |
C7—H7 | 0.9900 | C23—H23A | 0.9800 |
C8—C9 | 1.545 (5) | C23—H23B | 0.9800 |
C8—H8A | 0.9800 | C24—H24A | 0.9800 |
C8—H8B | 0.9800 | C24—H24B | 0.9800 |
C9—C10 | 1.534 (5) | | |
| | | |
N5i—Cd1—N5ii | 180.0 | C12—C11—H11A | 109.9 |
N5i—Cd1—O1 | 90.16 (10) | C5—C11—H11B | 109.9 |
N5ii—Cd1—O1 | 89.84 (10) | C12—C11—H11B | 109.9 |
N5i—Cd1—O1iii | 89.84 (10) | H11A—C11—H11B | 108.3 |
N5ii—Cd1—O1iii | 90.16 (10) | C13—C12—C11 | 110.0 (4) |
O1—Cd1—O1iii | 180.00 (4) | C13—C12—C14 | 109.9 (4) |
N5i—Cd1—N1iii | 91.75 (12) | C11—C12—C14 | 109.9 (4) |
N5ii—Cd1—N1iii | 88.25 (12) | C13—C12—H12 | 109.0 |
O1—Cd1—N1iii | 83.96 (9) | C11—C12—H12 | 109.0 |
O1iii—Cd1—N1iii | 96.04 (9) | C14—C12—H12 | 109.0 |
N5i—Cd1—N1 | 88.25 (12) | C12—C13—C7 | 108.4 (4) |
N5ii—Cd1—N1 | 91.75 (12) | C12—C13—H13A | 110.0 |
O1—Cd1—N1 | 96.04 (9) | C7—C13—H13A | 110.0 |
O1iii—Cd1—N1 | 83.96 (9) | C12—C13—H13B | 110.0 |
N1iii—Cd1—N1 | 180.0 | C7—C13—H13B | 110.0 |
Cd1—O1—H1W | 109.8 | H13A—C13—H13B | 108.4 |
Cd1—O1—H2W | 114.9 | C12—C14—C9 | 111.7 (3) |
H1W—O1—H2W | 108.5 | C12—C14—H14A | 109.3 |
H3W—O2—H4W | 108.5 | C9—C14—H14A | 109.3 |
C1—N1—N2 | 106.6 (3) | C12—C14—H14B | 109.3 |
C1—N1—Cd1 | 126.2 (3) | C9—C14—H14B | 109.3 |
N2—N1—Cd1 | 126.8 (3) | H14A—C14—H14B | 107.9 |
C2—N2—N1 | 106.8 (3) | N6—C15—C16 | 109.2 (3) |
C1—N3—C2 | 103.6 (3) | N6—C15—C21 | 108.6 (3) |
C1—N3—C5 | 127.2 (3) | C16—C15—C21 | 109.9 (3) |
C2—N3—C5 | 129.2 (3) | N6—C15—C20 | 109.2 (3) |
C3—N4—N5 | 105.6 (3) | C16—C15—C20 | 109.8 (3) |
C4—N5—N4 | 107.5 (3) | C21—C15—C20 | 110.1 (3) |
C4—N5—Cd1iv | 129.0 (3) | C15—C16—C17 | 108.0 (3) |
N4—N5—Cd1iv | 123.1 (3) | C15—C16—H16A | 110.1 |
C4—N6—C3 | 104.0 (3) | C17—C16—H16A | 110.1 |
C4—N6—C15 | 129.3 (3) | C15—C16—H16B | 110.1 |
C3—N6—C15 | 126.7 (3) | C17—C16—H16B | 110.1 |
N1—C1—N3 | 111.6 (4) | H16A—C16—H16B | 108.4 |
N1—C1—H1 | 124.2 | C18—C17—C16 | 110.2 (4) |
N3—C1—H1 | 124.2 | C18—C17—C23 | 108.9 (4) |
N2—C2—N3 | 111.5 (4) | C16—C17—C23 | 110.8 (4) |
N2—C2—H2 | 124.3 | C18—C17—H17 | 109.0 |
N3—C2—H2 | 124.3 | C16—C17—H17 | 109.0 |
N4—C3—N6 | 112.3 (4) | C23—C17—H17 | 109.0 |
N4—C3—H3 | 123.9 | C19—C18—C17 | 109.1 (4) |
N6—C3—H3 | 123.9 | C19—C18—H18A | 109.9 |
N5—C4—N6 | 110.6 (4) | C17—C18—H18A | 109.9 |
N5—C4—H4 | 124.7 | C19—C18—H18B | 109.9 |
N6—C4—H4 | 124.7 | C17—C18—H18B | 109.9 |
N3—C5—C11 | 109.1 (3) | H18A—C18—H18B | 108.3 |
N3—C5—C6 | 110.2 (3) | C18—C19—C24 | 110.9 (4) |
C11—C5—C6 | 109.6 (4) | C18—C19—C20 | 109.2 (4) |
N3—C5—C10 | 109.3 (3) | C24—C19—C20 | 109.5 (3) |
C11—C5—C10 | 109.5 (3) | C18—C19—H19 | 109.1 |
C6—C5—C10 | 109.1 (3) | C24—C19—H19 | 109.1 |
C5—C6—C7 | 109.2 (3) | C20—C19—H19 | 109.1 |
C5—C6—H6A | 109.8 | C15—C20—C19 | 108.2 (3) |
C7—C6—H6A | 109.8 | C15—C20—H20A | 110.1 |
C5—C6—H6B | 109.8 | C19—C20—H20A | 110.1 |
C7—C6—H6B | 109.8 | C15—C20—H20B | 110.1 |
H6A—C6—H6B | 108.3 | C19—C20—H20B | 110.1 |
C6—C7—C13 | 109.9 (4) | H20A—C20—H20B | 108.4 |
C6—C7—C8 | 109.0 (4) | C15—C21—C22 | 111.4 (3) |
C13—C7—C8 | 110.3 (4) | C15—C21—H21A | 109.3 |
C6—C7—H7 | 109.2 | C22—C21—H21A | 109.3 |
C13—C7—H7 | 109.2 | C15—C21—H21B | 109.3 |
C8—C7—H7 | 109.2 | C22—C21—H21B | 109.3 |
C7—C8—C9 | 111.1 (3) | H21A—C21—H21B | 108.0 |
C7—C8—H8A | 109.4 | C23—C22—C21 | 108.0 (3) |
C9—C8—H8A | 109.4 | C23—C22—C24 | 107.3 (3) |
C7—C8—H8B | 109.4 | C21—C22—C24 | 107.2 (3) |
C9—C8—H8B | 109.4 | C23—C22—C9 | 110.7 (3) |
H8A—C8—H8B | 108.0 | C21—C22—C9 | 111.5 (3) |
C10—C9—C14 | 107.4 (3) | C24—C22—C9 | 112.0 (3) |
C10—C9—C8 | 107.2 (3) | C22—C23—C17 | 110.7 (4) |
C14—C9—C8 | 107.3 (3) | C22—C23—H23A | 109.5 |
C10—C9—C22 | 111.5 (3) | C17—C23—H23A | 109.5 |
C14—C9—C22 | 111.8 (3) | C22—C23—H23B | 109.5 |
C8—C9—C22 | 111.4 (3) | C17—C23—H23B | 109.5 |
C9—C10—C5 | 111.8 (3) | H23A—C23—H23B | 108.1 |
C9—C10—H10A | 109.3 | C19—C24—C22 | 111.1 (3) |
C5—C10—H10A | 109.3 | C19—C24—H24A | 109.4 |
C9—C10—H10B | 109.3 | C22—C24—H24A | 109.4 |
C5—C10—H10B | 109.3 | C19—C24—H24B | 109.4 |
H10A—C10—H10B | 107.9 | C22—C24—H24B | 109.4 |
C5—C11—C12 | 108.9 (3) | H24A—C24—H24B | 108.0 |
C5—C11—H11A | 109.9 | N7—C25—Se1 | 178.6 (6) |
| | | |
N5i—Cd1—N1—C1 | 150.7 (4) | C14—C12—C13—C7 | −60.3 (4) |
N5ii—Cd1—N1—C1 | −29.3 (4) | C6—C7—C13—C12 | −60.3 (5) |
O1—Cd1—N1—C1 | 60.8 (4) | C8—C7—C13—C12 | 59.9 (5) |
O1iii—Cd1—N1—C1 | −119.2 (4) | C13—C12—C14—C9 | 61.2 (4) |
N5i—Cd1—N1—N2 | −37.1 (4) | C11—C12—C14—C9 | −60.0 (5) |
N5ii—Cd1—N1—N2 | 142.9 (4) | C10—C9—C14—C12 | 57.2 (4) |
O1—Cd1—N1—N2 | −127.1 (3) | C8—C9—C14—C12 | −57.8 (4) |
O1iii—Cd1—N1—N2 | 52.9 (3) | C22—C9—C14—C12 | 179.8 (3) |
C1—N1—N2—C2 | −0.8 (5) | C4—N6—C15—C16 | −4.0 (6) |
Cd1—N1—N2—C2 | −174.2 (3) | C3—N6—C15—C16 | 177.8 (4) |
C3—N4—N5—C4 | −0.1 (5) | C4—N6—C15—C21 | −123.8 (4) |
C3—N4—N5—Cd1iv | −173.6 (3) | C3—N6—C15—C21 | 58.0 (5) |
N2—N1—C1—N3 | 0.4 (5) | C4—N6—C15—C20 | 116.1 (5) |
Cd1—N1—C1—N3 | 173.9 (3) | C3—N6—C15—C20 | −62.1 (5) |
C2—N3—C1—N1 | 0.1 (5) | N6—C15—C16—C17 | −179.5 (3) |
C5—N3—C1—N1 | 178.4 (4) | C21—C15—C16—C17 | −60.5 (4) |
N1—N2—C2—N3 | 0.8 (6) | C20—C15—C16—C17 | 60.8 (5) |
C1—N3—C2—N2 | −0.6 (5) | C15—C16—C17—C18 | −60.4 (5) |
C5—N3—C2—N2 | −178.8 (4) | C15—C16—C17—C23 | 60.2 (5) |
N5—N4—C3—N6 | 0.1 (5) | C16—C17—C18—C19 | 61.2 (5) |
C4—N6—C3—N4 | 0.0 (5) | C23—C17—C18—C19 | −60.5 (5) |
C15—N6—C3—N4 | 178.5 (4) | C17—C18—C19—C24 | 59.6 (5) |
N4—N5—C4—N6 | 0.0 (5) | C17—C18—C19—C20 | −61.1 (5) |
Cd1iv—N5—C4—N6 | 173.1 (3) | N6—C15—C20—C19 | 178.9 (3) |
C3—N6—C4—N5 | 0.0 (5) | C16—C15—C20—C19 | −61.4 (4) |
C15—N6—C4—N5 | −178.5 (4) | C21—C15—C20—C19 | 59.7 (4) |
C1—N3—C5—C11 | 43.0 (6) | C18—C19—C20—C15 | 61.0 (5) |
C2—N3—C5—C11 | −139.1 (5) | C24—C19—C20—C15 | −60.5 (5) |
C1—N3—C5—C6 | 163.3 (4) | N6—C15—C21—C22 | −179.6 (3) |
C2—N3—C5—C6 | −18.8 (6) | C16—C15—C21—C22 | 61.0 (4) |
C1—N3—C5—C10 | −76.7 (5) | C20—C15—C21—C22 | −60.1 (4) |
C2—N3—C5—C10 | 101.2 (5) | C15—C21—C22—C23 | −57.6 (4) |
N3—C5—C6—C7 | −179.8 (3) | C15—C21—C22—C24 | 57.7 (4) |
C11—C5—C6—C7 | −59.8 (4) | C15—C21—C22—C9 | −179.4 (3) |
C10—C5—C6—C7 | 60.2 (4) | C10—C9—C22—C23 | 166.6 (3) |
C5—C6—C7—C13 | 59.9 (5) | C14—C9—C22—C23 | 46.4 (4) |
C5—C6—C7—C8 | −61.0 (4) | C8—C9—C22—C23 | −73.6 (4) |
C6—C7—C8—C9 | 61.2 (4) | C10—C9—C22—C21 | −73.2 (4) |
C13—C7—C8—C9 | −59.6 (4) | C14—C9—C22—C21 | 166.6 (3) |
C7—C8—C9—C10 | −58.4 (4) | C8—C9—C22—C21 | 46.6 (4) |
C7—C8—C9—C14 | 56.7 (4) | C10—C9—C22—C24 | 46.9 (4) |
C7—C8—C9—C22 | 179.3 (3) | C14—C9—C22—C24 | −73.3 (4) |
C14—C9—C10—C5 | −57.2 (4) | C8—C9—C22—C24 | 166.7 (3) |
C8—C9—C10—C5 | 57.8 (4) | C21—C22—C23—C17 | 56.4 (4) |
C22—C9—C10—C5 | −179.9 (3) | C24—C22—C23—C17 | −58.9 (4) |
N3—C5—C10—C9 | 179.5 (3) | C9—C22—C23—C17 | 178.7 (3) |
C11—C5—C10—C9 | 60.0 (4) | C18—C17—C23—C22 | 61.8 (5) |
C6—C5—C10—C9 | −59.9 (4) | C16—C17—C23—C22 | −59.5 (5) |
N3—C5—C11—C12 | −179.1 (3) | C18—C19—C24—C22 | −58.8 (5) |
C6—C5—C11—C12 | 60.1 (5) | C20—C19—C24—C22 | 61.7 (5) |
C10—C5—C11—C12 | −59.6 (4) | C23—C22—C24—C19 | 57.1 (4) |
C5—C11—C12—C13 | −61.2 (5) | C21—C22—C24—C19 | −58.7 (4) |
C5—C11—C12—C14 | 60.0 (5) | C9—C22—C24—C19 | 178.8 (3) |
C11—C12—C13—C7 | 60.9 (5) | | |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) x−1, −y+1/2, z−1/2; (iii) −x, −y+1, −z; (iv) −x+1, y−1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1W···O2 | 0.85 | 1.86 | 2.703 (4) | 170 |
O1—H2W···N2v | 0.85 | 2.08 | 2.909 (4) | 163 |
O2—H3W···Se1v | 0.85 | 2.47 | 3.321 (2) | 174 |
O2—H4W···N7 | 0.85 | 1.99 | 2.821 (6) | 166 |
C1—H1···N4ii | 0.94 | 2.44 | 3.109 (5) | 128 |
C2—H2···O2vi | 0.94 | 2.64 | 3.438 (5) | 143 |
C3—H3···Se1 | 0.94 | 2.86 | 3.646 (4) | 142 |
Symmetry codes: (ii) x−1, −y+1/2, z−1/2; (v) x−1, y, z; (vi) x+1, y, z. |
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