In the crystal structure of the title complex, [Cd(C
2N
3)
2(C
8H
10N
4)]
n or [Cd(dca)
2(bim)]
n, where dca is dicyanamide and bim is 1,2-bis(imidazol-1-yl)ethane, each Cd
II atom is in a distorted octahedral environment. Four N atoms from four dca ligands occupy the equatorial positions, and two N atoms from two bim ligands occupy the axial positions. Each Cd
II atom is situated at a center of symmetry, and a twofold axis runs through the mid-points of the bim exocyclic C—C bond and the Cd
Cd vector. The structure consists of chains in which neighboring Cd
II atoms are connected through one bim and two end-to-end dca bridges.
Supporting information
CCDC reference: 294026
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (C-C) = 0.004 Å
- Disorder in main residue
- R factor = 0.020
- wR factor = 0.054
- Data-to-parameter ratio = 12.3
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT301_ALERT_3_C Main Residue Disorder ......................... 8.00 Perc.
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
catena-poly[cadmium(II)-µ-1,2-bis(imidazol-1-yl)ethane-
κ2N3:
N3'–
di-µ-1,5-dicyanamido-
κ4N1:
N5]
top
Crystal data top
[Cd(C2N3)2(C8H10N4)] | F(000) = 800 |
Mr = 406.71 | Dx = 1.736 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3014 reflections |
a = 12.770 (3) Å | θ = 3.1–25.4° |
b = 8.4986 (17) Å | µ = 1.42 mm−1 |
c = 14.568 (3) Å | T = 193 K |
β = 100.162 (6)° | Block, colorless |
V = 1556.2 (6) Å3 | 0.40 × 0.30 × 0.11 mm |
Z = 4 | |
Data collection top
Rigaku Mercury CCD diffractometer | 1424 independent reflections |
Radiation source: fine-focus sealed tube | 1339 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
ω scans | θmax = 25.3°, θmin = 3.1° |
Absorption correction: multi-scan (North et al., 1968) | h = −15→15 |
Tmin = 0.601, Tmax = 0.860 | k = −9→10 |
7367 measured reflections | l = −17→17 |
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)] = 0.020 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0312P)2 + 1.619P] where P = (Fo2 + 2Fc2)/3 |
1424 reflections | (Δ/σ)max < 0.001 |
116 parameters | Δρmax = 0.37 e Å−3 |
0 restraints | Δρmin = −0.36 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 >
2σ(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 | Occ. (<1) |
Cd1 | 0.5000 | 0.5000 | 0.5000 | 0.02520 (10) | |
N1 | 0.48122 (13) | 0.0401 (2) | 0.63851 (12) | 0.0248 (3) | |
N2 | 0.46656 (13) | 0.2588 (2) | 0.55640 (12) | 0.0295 (4) | |
N3 | 0.62292 (16) | 0.5463 (3) | 0.63574 (14) | 0.0392 (4) | |
N4A | 0.7229 (8) | 0.5469 (13) | 0.7973 (7) | 0.053 (3) | 0.50 |
N4B | 0.7206 (8) | 0.6142 (11) | 0.7873 (8) | 0.045 (2) | 0.50 |
N5 | 0.64184 (15) | 0.6042 (2) | 0.93115 (13) | 0.0386 (4) | |
C1 | 0.52394 (16) | 0.1813 (2) | 0.62616 (14) | 0.0280 (4) | |
H1A | 0.5875 | 0.2204 | 0.6630 | 0.034* | |
C2 | 0.38269 (16) | 0.1612 (3) | 0.52245 (15) | 0.0339 (5) | |
H2A | 0.3275 | 0.1852 | 0.4716 | 0.041* | |
C3 | 0.39044 (19) | 0.0258 (3) | 0.57227 (18) | 0.0326 (5) | |
H3A | 0.3430 | −0.0611 | 0.5633 | 0.039* | |
C4 | 0.52426 (16) | −0.0809 (2) | 0.70589 (14) | 0.0272 (4) | |
H4A | 0.6021 | −0.0654 | 0.7234 | 0.033* | |
H4B | 0.5123 | −0.1852 | 0.6757 | 0.033* | |
C5 | 0.66585 (16) | 0.5622 (3) | 0.71016 (16) | 0.0348 (5) | |
C6 | 0.67607 (16) | 0.5910 (3) | 0.86445 (15) | 0.0341 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.03254 (15) | 0.02412 (15) | 0.01858 (14) | −0.00034 (7) | 0.00357 (9) | 0.00068 (7) |
N1 | 0.0253 (8) | 0.0255 (8) | 0.0234 (9) | 0.0006 (7) | 0.0032 (7) | −0.0005 (7) |
N2 | 0.0314 (8) | 0.0272 (9) | 0.0299 (9) | −0.0002 (7) | 0.0049 (7) | 0.0018 (7) |
N3 | 0.0431 (11) | 0.0460 (11) | 0.0259 (11) | −0.0018 (10) | −0.0011 (9) | −0.0028 (9) |
N4A | 0.027 (3) | 0.112 (7) | 0.019 (3) | 0.028 (5) | 0.001 (2) | 0.003 (5) |
N4B | 0.025 (3) | 0.083 (6) | 0.025 (3) | −0.012 (4) | −0.003 (2) | 0.004 (4) |
N5 | 0.0410 (10) | 0.0431 (11) | 0.0336 (10) | −0.0043 (8) | 0.0115 (9) | −0.0005 (8) |
C1 | 0.0274 (10) | 0.0250 (10) | 0.0304 (10) | −0.0016 (8) | 0.0018 (8) | −0.0003 (8) |
C2 | 0.0283 (10) | 0.0377 (12) | 0.0333 (12) | −0.0025 (9) | −0.0012 (9) | 0.0036 (9) |
C3 | 0.0289 (11) | 0.0352 (11) | 0.0318 (12) | −0.0065 (9) | −0.0002 (9) | 0.0008 (9) |
C4 | 0.0288 (10) | 0.0212 (9) | 0.0308 (11) | 0.0026 (8) | 0.0025 (8) | −0.0002 (8) |
C5 | 0.0257 (10) | 0.0469 (14) | 0.0325 (13) | 0.0032 (10) | 0.0072 (10) | −0.0030 (11) |
C6 | 0.0231 (10) | 0.0471 (14) | 0.0297 (12) | 0.0008 (9) | −0.0020 (9) | −0.0017 (10) |
Geometric parameters (Å, º) top
Cd1—N2i | 2.2769 (17) | N4A—C5 | 1.353 (10) |
Cd1—N2 | 2.2769 (17) | N4B—C5 | 1.292 (11) |
Cd1—N3 | 2.331 (2) | N4B—C6 | 1.360 (11) |
Cd1—N3i | 2.331 (2) | N5—C6 | 1.139 (3) |
Cd1—N5ii | 2.3900 (19) | N5—Cd1iii | 2.3900 (19) |
Cd1—N5iii | 2.3900 (19) | C1—H1A | 0.9500 |
N1—C1 | 1.343 (3) | C2—C3 | 1.355 (3) |
N1—C3 | 1.377 (3) | C2—H2A | 0.9500 |
N1—C4 | 1.460 (3) | C3—H3A | 0.9500 |
N2—C1 | 1.319 (3) | C4—C4iii | 1.522 (4) |
N2—C2 | 1.375 (3) | C4—H4A | 0.9900 |
N3—C5 | 1.133 (3) | C4—H4B | 0.9900 |
N4A—C6 | 1.290 (11) | | |
| | | |
N2i—Cd1—N2 | 180.0 | C6—N4A—C5 | 116.0 (7) |
N2i—Cd1—N3 | 90.74 (7) | C5—N4B—C6 | 115.3 (7) |
N2—Cd1—N3 | 89.26 (7) | C6—N5—Cd1iii | 139.01 (18) |
N2i—Cd1—N3i | 89.26 (7) | N2—C1—N1 | 111.44 (18) |
N2—Cd1—N3i | 90.74 (7) | N2—C1—H1A | 124.3 |
N3—Cd1—N3i | 180.0 | N1—C1—H1A | 124.3 |
N2i—Cd1—N5ii | 88.74 (6) | C3—C2—N2 | 109.92 (19) |
N2—Cd1—N5ii | 91.26 (6) | C3—C2—H2A | 125.0 |
N3—Cd1—N5ii | 88.39 (7) | N2—C2—H2A | 125.0 |
N3i—Cd1—N5ii | 91.61 (7) | C2—C3—N1 | 105.86 (19) |
N2i—Cd1—N5iii | 91.26 (6) | C2—C3—H3A | 127.1 |
N2—Cd1—N5iii | 88.74 (6) | N1—C3—H3A | 127.1 |
N3—Cd1—N5iii | 91.61 (7) | N1—C4—C4iii | 113.99 (15) |
N3i—Cd1—N5iii | 88.39 (7) | N1—C4—H4A | 108.8 |
N5ii—Cd1—N5iii | 180.0 | C4iii—C4—H4A | 108.8 |
C1—N1—C3 | 107.27 (18) | N1—C4—H4B | 108.8 |
C1—N1—C4 | 127.25 (17) | C4iii—C4—H4B | 108.8 |
C3—N1—C4 | 125.41 (18) | H4A—C4—H4B | 107.6 |
C1—N2—C2 | 105.51 (17) | N3—C5—N4B | 165.7 (4) |
C1—N2—Cd1 | 127.83 (14) | N3—C5—N4A | 167.1 (5) |
C2—N2—Cd1 | 126.64 (14) | N5—C6—N4A | 167.2 (5) |
C5—N3—Cd1 | 166.24 (19) | N5—C6—N4B | 165.8 (5) |
| | | |
N3—Cd1—N2—C1 | −15.63 (18) | C1—N1—C3—C2 | 0.0 (3) |
N3i—Cd1—N2—C1 | 164.37 (18) | C4—N1—C3—C2 | −177.24 (19) |
N5ii—Cd1—N2—C1 | 72.74 (18) | C1—N1—C4—C4iii | 98.1 (2) |
N5iii—Cd1—N2—C1 | −107.26 (18) | C3—N1—C4—C4iii | −85.3 (3) |
N3—Cd1—N2—C2 | 166.29 (18) | Cd1—N3—C5—N4B | −126 (2) |
N3i—Cd1—N2—C2 | −13.71 (18) | Cd1—N3—C5—N4A | 93 (2) |
N5ii—Cd1—N2—C2 | −105.34 (18) | N4A—N4B—C5—N3 | −161.2 (11) |
N5iii—Cd1—N2—C2 | 74.66 (18) | C6—N4B—C5—N3 | 134.3 (18) |
N2i—Cd1—N3—C5 | 124.7 (9) | C6—N4B—C5—N4A | −64.5 (17) |
N2—Cd1—N3—C5 | −55.3 (9) | N4B—N4A—C5—N3 | 159.0 (14) |
N5ii—Cd1—N3—C5 | −146.6 (9) | C6—N4A—C5—N3 | −127.7 (19) |
N5iii—Cd1—N3—C5 | 33.4 (9) | C6—N4A—C5—N4B | 73 (2) |
C6—N4A—N4B—C5 | −120.1 (4) | Cd1iii—N5—C6—N4A | −75 (3) |
C5—N4A—N4B—C6 | 120.1 (4) | Cd1iii—N5—C6—N4B | 142.2 (19) |
C2—N2—C1—N1 | −0.1 (2) | N4B—N4A—C6—N5 | −160.0 (13) |
Cd1—N2—C1—N1 | −178.47 (13) | C5—N4A—C6—N5 | 134 (2) |
C3—N1—C1—N2 | 0.1 (2) | C5—N4A—C6—N4B | −65.9 (16) |
C4—N1—C1—N2 | 177.20 (18) | N4A—N4B—C6—N5 | 162.0 (12) |
C1—N2—C2—C3 | 0.0 (3) | C5—N4B—C6—N5 | −126.1 (16) |
Cd1—N2—C2—C3 | 178.47 (15) | C5—N4B—C6—N4A | 71.9 (19) |
N2—C2—C3—N1 | 0.0 (3) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, −y+1, z−1/2; (iii) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C4—H4A···N4Aiv | 0.99 | 2.50 | 3.414 (10) | 154 |
Symmetry code: (iv) −x+3/2, y−1/2, −z+3/2. |