Buy article online - an online subscription or single-article purchase is required to access this article.
In the title compound, [Cd(C
4H
13N
3)
2](C
10H
6O
6S
2), the Cd atom, located on an inversion centre, is six-coordinated by two diethylenetriamine ligands. The anion is centrosymmetric. The metal complex cations are connected to naphthalene-1,5-disulfonate anions
via weak self-complementary N—H
O hydrogen bonds into two-dimensional extended sheets, which are further linked into three-dimensional networks with channels along the
a axis.
Supporting information
CCDC reference: 642969
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.003 Å
- R factor = 0.028
- wR factor = 0.079
- Data-to-parameter ratio = 21.3
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94
Alert level C
REFLT03_ALERT_3_C Reflection count < 95% complete
From the CIF: _diffrn_reflns_theta_max 29.99
From the CIF: _diffrn_reflns_theta_full 29.99
From the CIF: _reflns_number_total 3217
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 3409
Completeness (_total/calc) 94.37%
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ?
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3
PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2 ... ?
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
4 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97, enCIFer (Allen et al., 2004) and publCIF (Westrip,
2007).
Bis(
N,
N',
N''-diethylenetriamine-
κ3N)cadmium(II)
naphthalene-1,5-disulfonate
top
Crystal data top
[Cd(C4H13N3)2](C10H6O6S2) | Z = 1 |
Mr = 605.02 | F(000) = 310 |
Triclinic, P1 | Dx = 1.713 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.0675 (1) Å | Cell parameters from 4029 reflections |
b = 8.8907 (1) Å | θ = 12–18° |
c = 9.9507 (2) Å | µ = 1.16 mm−1 |
α = 110.732 (3)° | T = 273 K |
β = 90.730 (2)° | Block, colourless |
γ = 116.218 (2)° | 0.35 × 0.30 × 0.20 mm |
V = 586.54 (3) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 3217 independent reflections |
Radiation source: fine-focus sealed tube | 2994 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
ω scans | θmax = 30.0°, θmin = 4.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→10 |
Tmin = 0.674, Tmax = 0.793 | k = −12→12 |
4209 measured reflections | l = −13→8 |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.079 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0548P)2 + 0.0328P] where P = (Fo2 + 2Fc2)/3 |
3217 reflections | (Δ/σ)max < 0.001 |
151 parameters | Δρmax = 0.72 e Å−3 |
0 restraints | Δρmin = −0.72 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 | 0.5000 | 0.5000 | 0.5000 | 0.03225 (8) | |
S1 | 0.79889 (6) | 0.06124 (6) | 0.30487 (4) | 0.02934 (10) | |
O1 | 0.6051 (2) | −0.0563 (3) | 0.22474 (18) | 0.0479 (4) | |
O2 | 0.8362 (2) | 0.0263 (2) | 0.43086 (16) | 0.0442 (3) | |
O3 | 0.8623 (3) | 0.2542 (2) | 0.34146 (18) | 0.0479 (4) | |
N1 | 0.5468 (3) | 0.2702 (3) | 0.5332 (2) | 0.0463 (4) | |
H1A | 0.4431 | 0.1918 | 0.5529 | 0.056* | |
H1B | 0.5756 | 0.2072 | 0.4528 | 0.056* | |
N2 | 0.6091 (2) | 0.6136 (2) | 0.75636 (19) | 0.0391 (4) | |
H2 | 0.7138 | 0.7247 | 0.7850 | 0.047* | |
N3 | 0.2194 (2) | 0.4244 (3) | 0.60111 (19) | 0.0406 (4) | |
H3A | 0.1631 | 0.4876 | 0.5890 | 0.049* | |
H3B | 0.1381 | 0.3042 | 0.5538 | 0.049* | |
C1 | 0.7060 (4) | 0.3729 (4) | 0.6593 (3) | 0.0579 (7) | |
H1C | 0.8181 | 0.4506 | 0.6335 | 0.070* | |
H1D | 0.7314 | 0.2879 | 0.6841 | 0.070* | |
C2 | 0.6610 (4) | 0.4894 (4) | 0.7908 (3) | 0.0543 (6) | |
H2A | 0.5575 | 0.4103 | 0.8229 | 0.065* | |
H2B | 0.7700 | 0.5613 | 0.8708 | 0.065* | |
C3 | 0.4594 (3) | 0.6397 (3) | 0.8277 (2) | 0.0471 (5) | |
H3C | 0.4542 | 0.7431 | 0.8194 | 0.057* | |
H3D | 0.4885 | 0.6668 | 0.9311 | 0.057* | |
C4 | 0.2681 (3) | 0.4690 (3) | 0.7573 (2) | 0.0445 (5) | |
H4A | 0.2715 | 0.3668 | 0.7694 | 0.053* | |
H4B | 0.1721 | 0.4894 | 0.8062 | 0.053* | |
C5 | 0.9428 (2) | 0.0049 (2) | 0.18365 (17) | 0.0236 (3) | |
C6 | 0.9397 (2) | 0.0218 (2) | 0.04607 (17) | 0.0230 (3) | |
C7 | 1.0603 (2) | −0.0505 (2) | 0.22731 (18) | 0.0284 (3) | |
H7 | 1.0621 | −0.0592 | 0.3177 | 0.034* | |
C8 | 1.1782 (3) | −0.0943 (3) | 0.1354 (2) | 0.0319 (3) | |
H8 | 1.2567 | −0.1327 | 0.1654 | 0.038* | |
C9 | 1.1782 (2) | −0.0809 (2) | 0.00269 (19) | 0.0280 (3) | |
H9 | 1.2565 | −0.1107 | −0.0566 | 0.034* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.03525 (11) | 0.03580 (11) | 0.03281 (11) | 0.01865 (8) | 0.01277 (7) | 0.01891 (8) |
S1 | 0.0298 (2) | 0.0365 (2) | 0.02606 (19) | 0.01774 (17) | 0.01185 (16) | 0.01449 (17) |
O1 | 0.0265 (6) | 0.0685 (10) | 0.0468 (8) | 0.0188 (7) | 0.0125 (6) | 0.0260 (8) |
O2 | 0.0512 (8) | 0.0661 (10) | 0.0322 (7) | 0.0344 (8) | 0.0206 (6) | 0.0289 (7) |
O3 | 0.0665 (10) | 0.0409 (8) | 0.0443 (8) | 0.0334 (8) | 0.0230 (8) | 0.0149 (6) |
N1 | 0.0570 (11) | 0.0460 (10) | 0.0601 (11) | 0.0343 (9) | 0.0350 (9) | 0.0336 (9) |
N2 | 0.0336 (8) | 0.0338 (8) | 0.0390 (8) | 0.0059 (6) | 0.0033 (6) | 0.0164 (7) |
N3 | 0.0321 (8) | 0.0435 (9) | 0.0409 (9) | 0.0129 (7) | 0.0096 (7) | 0.0179 (7) |
C1 | 0.0524 (13) | 0.0842 (18) | 0.0840 (19) | 0.0475 (14) | 0.0341 (13) | 0.0635 (16) |
C2 | 0.0523 (13) | 0.0620 (14) | 0.0536 (13) | 0.0205 (11) | 0.0017 (10) | 0.0378 (12) |
C3 | 0.0502 (12) | 0.0383 (10) | 0.0339 (10) | 0.0116 (9) | 0.0087 (9) | 0.0067 (8) |
C4 | 0.0393 (10) | 0.0455 (11) | 0.0407 (10) | 0.0110 (9) | 0.0152 (8) | 0.0205 (9) |
C5 | 0.0222 (6) | 0.0244 (7) | 0.0239 (7) | 0.0098 (5) | 0.0062 (5) | 0.0109 (5) |
C6 | 0.0219 (6) | 0.0232 (7) | 0.0243 (7) | 0.0103 (6) | 0.0050 (6) | 0.0107 (5) |
C7 | 0.0303 (8) | 0.0333 (8) | 0.0273 (7) | 0.0154 (7) | 0.0074 (6) | 0.0178 (6) |
C8 | 0.0331 (8) | 0.0402 (9) | 0.0361 (9) | 0.0232 (7) | 0.0094 (7) | 0.0222 (7) |
C9 | 0.0288 (7) | 0.0335 (8) | 0.0304 (8) | 0.0200 (7) | 0.0099 (6) | 0.0154 (6) |
Geometric parameters (Å, º) top
Cd1—N1 | 2.3623 (18) | C1—H1D | 0.9700 |
Cd1—N2 | 2.3739 (17) | C2—H2A | 0.9700 |
Cd1—N3 | 2.4043 (17) | C2—H2B | 0.9700 |
S1—O1 | 1.4513 (15) | C3—C4 | 1.525 (3) |
S1—O2 | 1.4519 (15) | C3—H3C | 0.9700 |
S1—O3 | 1.4544 (16) | C3—H3D | 0.9700 |
S1—C5 | 1.7822 (16) | C4—H4A | 0.9700 |
N1—C1 | 1.474 (4) | C4—H4B | 0.9700 |
N1—H1A | 0.9000 | C5—C7 | 1.372 (2) |
N1—H1B | 0.9000 | C5—C6 | 1.430 (2) |
N2—C3 | 1.473 (3) | C6—C9i | 1.423 (2) |
N2—C2 | 1.478 (3) | C6—C6i | 1.428 (3) |
N2—H2 | 0.9100 | C7—C8 | 1.411 (2) |
N3—C4 | 1.462 (3) | C7—H7 | 0.9300 |
N3—H3A | 0.9000 | C8—C9 | 1.368 (2) |
N3—H3B | 0.9000 | C8—H8 | 0.9300 |
C1—C2 | 1.517 (4) | C9—H9 | 0.9300 |
C1—H1C | 0.9700 | | |
| | | |
N1ii—Cd1—N2 | 104.96 (7) | C2—C1—H1D | 109.6 |
N1—Cd1—N2 | 75.04 (7) | H1C—C1—H1D | 108.1 |
N1ii—Cd1—N3ii | 92.70 (7) | N2—C2—C1 | 111.93 (18) |
N1—Cd1—N3ii | 87.30 (6) | N2—C2—H2A | 109.2 |
N2—Cd1—N3ii | 104.99 (6) | C1—C2—H2A | 109.2 |
N1—Cd1—N3 | 92.70 (6) | N2—C2—H2B | 109.2 |
N2—Cd1—N3 | 75.01 (6) | C1—C2—H2B | 109.2 |
O1—S1—O2 | 112.82 (10) | H2A—C2—H2B | 107.9 |
O1—S1—O3 | 113.14 (11) | N2—C3—C4 | 111.01 (18) |
O2—S1—O3 | 112.61 (10) | N2—C3—H3C | 109.4 |
O1—S1—C5 | 106.62 (9) | C4—C3—H3C | 109.4 |
O2—S1—C5 | 105.82 (8) | N2—C3—H3D | 109.4 |
O3—S1—C5 | 105.04 (8) | C4—C3—H3D | 109.4 |
C1—N1—Cd1 | 103.83 (14) | H3C—C3—H3D | 108.0 |
C1—N1—H1A | 111.0 | N3—C4—C3 | 110.89 (17) |
Cd1—N1—H1A | 111.0 | N3—C4—H4A | 109.5 |
C1—N1—H1B | 111.0 | C3—C4—H4A | 109.5 |
Cd1—N1—H1B | 111.0 | N3—C4—H4B | 109.5 |
H1A—N1—H1B | 109.0 | C3—C4—H4B | 109.5 |
C3—N2—C2 | 114.43 (19) | H4A—C4—H4B | 108.0 |
C3—N2—Cd1 | 106.59 (13) | C7—C5—C6 | 120.85 (14) |
C2—N2—Cd1 | 110.47 (14) | C7—C5—S1 | 118.32 (12) |
C3—N2—H2 | 108.4 | C6—C5—S1 | 120.81 (11) |
C2—N2—H2 | 108.4 | C9i—C6—C6i | 118.63 (18) |
Cd1—N2—H2 | 108.4 | C9i—C6—C5 | 122.68 (14) |
C4—N3—Cd1 | 109.79 (13) | C6i—C6—C5 | 118.69 (17) |
C4—N3—H3A | 109.7 | C5—C7—C8 | 120.15 (15) |
Cd1—N3—H3A | 109.7 | C5—C7—H7 | 119.9 |
C4—N3—H3B | 109.7 | C8—C7—H7 | 119.9 |
Cd1—N3—H3B | 109.7 | C9—C8—C7 | 120.65 (15) |
H3A—N3—H3B | 108.2 | C9—C8—H8 | 119.7 |
N1—C1—C2 | 110.43 (18) | C7—C8—H8 | 119.7 |
N1—C1—H1C | 109.6 | C8—C9—C6i | 121.03 (15) |
C2—C1—H1C | 109.6 | C8—C9—H9 | 119.5 |
N1—C1—H1D | 109.6 | C6i—C9—H9 | 119.5 |
Symmetry codes: (i) −x+2, −y, −z; (ii) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O2iii | 0.90 | 2.29 | 3.181 (3) | 172 |
N1—H1B···O3 | 0.90 | 2.51 | 3.223 (2) | 137 |
N3—H3A···O3ii | 0.90 | 2.25 | 3.073 (2) | 151 |
N3—H3B···O2iv | 0.90 | 2.45 | 3.303 (2) | 158 |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) x−1, y, z. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.