metal-organic compounds
The title compound comprises centrosymmetric dimeric units, [Na2(PMDTA)2(H2O)2]2+ (PMDTA is N,N,N′,N′′,N′′-pentamethyldiethylenetriamine, C9H23N3), where two Na cations are bridged by two water molecules. Each Na+ cation is also coordinated by three N atoms of a PMDTA molecule to give a five-coordinate distorted square-pyramidal geometry. Polymeric chains are then obtained through weak interactions between the water molecules and the I− anions that provide the charge balance. The cations and anions lie on a mirror plane.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805021239/tk6237sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805021239/tk6237Isup2.hkl |
CCDC reference: 282682
Computing details top
Data collection: COLLECT (Nonius, 2001); cell refinement: DENZO/SCALEPACK; data reduction: DENZO/SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: CRYSTALS.
Di-µ-aqua-bis[{N-[(2-dimethylamino-κN)ethyl]-N,N',N'-trimethylethane-
1,2-diamine-κ2N,N'}sodium(I)] diiodide top
Crystal data top
[Na2(C9H23N3)2(H2O)2]I2 | F(000) = 688 |
Mr = 682.42 | Dx = 1.462 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2y | Cell parameters from 1809 reflections |
a = 13.7534 (6) Å | θ = 1–28° |
b = 17.1348 (8) Å | µ = 2.08 mm−1 |
c = 7.6723 (3) Å | T = 150 K |
β = 120.997 (2)° | Block, colorless |
V = 1549.87 (12) Å3 | 0.05 × 0.05 × 0.05 mm |
Z = 2 |
Data collection top
Nonius KappaCCD diffractometer | 1899 independent reflections |
Radiation source: sealed X-ray tube | 1629 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
ω scans | θmax = 27.9°, θmin = 2.1° |
Absorption correction: multi-scan DENZO/SCALEPACK (Otwinowski & Minor, 1997) | h = −17→18 |
Tmin = 0.901, Tmax = 0.901 | k = −22→20 |
3361 measured reflections | l = −10→10 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.040 | Only H-atom coordinates refined |
wR(F2) = 0.091 | Method, part 1, Chebychev polynomial (Watkin, 1994, Prince, 1982),
[weight] = 1.0/[A0T0(x) + A1T1(x) ··· + An-1Tn-1(x)] where Ai are the Chebychev coefficients listed below and x = F /Fmax. Method, robust weighting (Prince, 1982), W = [weight] [1-(δF/6 × σF)2]2. Ai are 25.3 38.1 24.1 10.0 3.69 |
S = 0.87 | (Δ/σ)max < 0.001 |
1629 reflections | Δρmax = 2.24 e Å−3 |
126 parameters | Δρmin = −0.72 e Å−3 |
58 restraints |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Na1 | 0.64595 (19) | 0.0000 | 0.1052 (4) | 0.0283 | |
O2 | 0.4804 (4) | 0.0000 | −0.2264 (6) | 0.0297 | |
N3 | 0.7401 (4) | 0.1284 (3) | 0.2278 (7) | 0.0435 | |
C4 | 0.8131 (6) | 0.1384 (4) | 0.1406 (11) | 0.0624 | |
C5 | 0.8794 (5) | 0.0691 (5) | 0.1577 (11) | 0.0645 | |
N6 | 0.8105 (5) | 0.0000 | 0.0548 (10) | 0.0393 | |
C7 | 0.7695 (7) | 0.0000 | −0.1612 (12) | 0.0468 | |
C8 | 0.8010 (5) | 0.1270 (4) | 0.4487 (9) | 0.0508 | |
C9 | 0.6633 (7) | 0.1946 (3) | 0.1583 (9) | 0.0595 | |
I10 | 0.5000 | 0.15724 (2) | 0.5000 | 0.0317 | |
H41 | 0.866 (2) | 0.1810 (15) | 0.212 (5) | 0.078 (2)* | |
H42 | 0.765 (2) | 0.1505 (19) | −0.005 (3) | 0.078 (2)* | |
H51 | 0.927 (3) | 0.0812 (16) | 0.101 (5) | 0.079 (2)* | |
H52 | 0.927 (3) | 0.0576 (16) | 0.304 (3) | 0.079 (2)* | |
H81 | 0.748 (2) | 0.126 (3) | 0.496 (4) | 0.062 (2)* | |
H82 | 0.847 (3) | 0.1728 (17) | 0.502 (4) | 0.062 (2)* | |
H83 | 0.849 (3) | 0.0818 (18) | 0.498 (4) | 0.062 (2)* | |
H91 | 0.614 (3) | 0.191 (2) | 0.212 (7) | 0.072 (2)* | |
H92 | 0.705 (2) | 0.2428 (13) | 0.203 (7) | 0.072 (2)* | |
H93 | 0.618 (3) | 0.194 (2) | 0.013 (3) | 0.072 (2)* | |
H5 | 0.7247 (14) | 0.0457 (8) | −0.222 (3) | 0.0579 (14)* | |
H12 | 0.832 (2) | 0.0000 | −0.182 (4) | 0.058 (2)* | |
H7 | 0.484 (5) | −0.038 (2) | −0.288 (8) | 0.0450 (14)* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Na1 | 0.0267 (11) | 0.0279 (11) | 0.0307 (12) | 0.0000 | 0.0152 (10) | 0.0000 |
O2 | 0.039 (2) | 0.028 (2) | 0.029 (2) | 0.0000 | 0.0215 (19) | 0.0000 |
N3 | 0.061 (3) | 0.038 (2) | 0.049 (2) | −0.020 (2) | 0.041 (2) | −0.0142 (19) |
C4 | 0.081 (4) | 0.063 (4) | 0.069 (4) | −0.039 (3) | 0.056 (4) | −0.029 (3) |
C5 | 0.047 (3) | 0.094 (5) | 0.069 (4) | −0.026 (3) | 0.042 (3) | −0.025 (4) |
N6 | 0.031 (3) | 0.044 (3) | 0.051 (3) | 0.0000 | 0.027 (3) | 0.0000 |
C7 | 0.041 (4) | 0.052 (4) | 0.049 (4) | 0.0000 | 0.024 (3) | 0.0000 |
C8 | 0.048 (3) | 0.060 (3) | 0.044 (3) | −0.012 (3) | 0.023 (2) | 0.000 (3) |
C9 | 0.093 (5) | 0.041 (3) | 0.044 (3) | −0.008 (3) | 0.035 (3) | 0.004 (2) |
I10 | 0.0374 (2) | 0.0282 (2) | 0.0317 (2) | 0.0000 | 0.01944 (16) | 0.0000 |
Geometric parameters (Å, º) top
Na1—O2i | 2.356 (5) | C5—N6 | 1.468 (7) |
Na1—N3ii | 2.480 (4) | C5—H51 | 0.977 (19) |
Na1—O2 | 2.385 (5) | C5—H52 | 0.983 (19) |
Na1—N3 | 2.480 (4) | N6—C7 | 1.450 (10) |
Na1—N6 | 2.485 (6) | C7—H5ii | 0.956 (14) |
O2—H7ii | 0.820 (14) | C7—H5 | 0.956 (14) |
O2—H7 | 0.820 (14) | C7—H12 | 0.959 (19) |
N3—C4 | 1.476 (7) | C8—H81 | 0.958 (19) |
N3—C8 | 1.453 (7) | C8—H82 | 0.959 (19) |
N3—C9 | 1.452 (8) | C8—H83 | 0.960 (19) |
C4—C5 | 1.461 (10) | C9—H91 | 0.961 (19) |
C4—H41 | 0.977 (19) | C9—H92 | 0.962 (19) |
C4—H42 | 0.984 (19) | C9—H93 | 0.959 (19) |
O2i—Na1—N3ii | 101.39 (12) | C4—C5—H51 | 108.6 (16) |
O2i—Na1—O2 | 85.87 (16) | N6—C5—H51 | 109.0 (16) |
N3ii—Na1—O2 | 115.45 (13) | C4—C5—H52 | 106.2 (16) |
O2i—Na1—N3 | 101.39 (12) | N6—C5—H52 | 108.4 (16) |
N3ii—Na1—N3 | 125.1 (3) | H51—C5—H52 | 110.6 (17) |
O2—Na1—N3 | 115.45 (13) | C5ii—N6—C5 | 107.6 (7) |
O2i—Na1—N6 | 167.9 (2) | C5ii—N6—Na1 | 107.7 (3) |
N3ii—Na1—N6 | 73.71 (13) | C5—N6—Na1 | 107.7 (3) |
O2—Na1—N6 | 106.2 (2) | C5ii—N6—C7 | 112.2 (4) |
N3—Na1—N6 | 73.71 (13) | C5—N6—C7 | 112.2 (4) |
Na1i—O2—Na1 | 94.13 (16) | Na1—N6—C7 | 109.2 (4) |
Na1i—O2—H7ii | 120 (4) | N6—C7—H5ii | 109.3 (11) |
Na1—O2—H7ii | 108 (4) | N6—C7—H5 | 109.3 (11) |
Na1i—O2—H7 | 120 (4) | H5ii—C7—H5 | 109.9 (17) |
Na1—O2—H7 | 108 (4) | N6—C7—H12 | 109.9 (17) |
H7ii—O2—H7 | 105 (8) | H5ii—C7—H12 | 109.2 (11) |
Na1—N3—C4 | 106.0 (3) | H5—C7—H12 | 109.2 (11) |
Na1—N3—C8 | 107.6 (3) | N3—C8—H81 | 110.2 (16) |
C4—N3—C8 | 114.4 (5) | N3—C8—H82 | 110.0 (16) |
Na1—N3—C9 | 114.5 (4) | H81—C8—H82 | 108.6 (17) |
C4—N3—C9 | 106.2 (5) | N3—C8—H83 | 110.0 (16) |
C8—N3—C9 | 108.3 (5) | H81—C8—H83 | 109.3 (17) |
N3—C4—C5 | 113.8 (5) | H82—C8—H83 | 108.8 (17) |
N3—C4—H41 | 108.6 (16) | N3—C9—H91 | 109.0 (17) |
C5—C4—H41 | 107.7 (16) | N3—C9—H92 | 110.6 (16) |
N3—C4—H42 | 109.2 (16) | H91—C9—H92 | 109.5 (17) |
C5—C4—H42 | 107.0 (16) | N3—C9—H93 | 109.2 (17) |
H41—C4—H42 | 110.5 (17) | H91—C9—H93 | 109.1 (17) |
C4—C5—N6 | 114.0 (5) | H92—C9—H93 | 109.4 (17) |
Symmetry codes: (i) −x+1, −y, −z; (ii) x, −y, z. |