Both of the title compounds,
catena-poly[[[tetraaquamagnesium(I)]-
-4,4'-bipyridine-
2N:
N'] diiodide bis(4,4'-bipyridine) solvate], {[Mg(C
10H
8N
2)(H
2O)
4]I
2·2C
10H
8N
2}
n, (I), and
catena-poly[[[
-4,4'-bipyridine-bis[diiodobis(propan-1-ol)strontium(I)]]-di-
-4,4'-bipyridine-
4N:
N'] bis(4,4'-bipyridine) solvate], {[Sr
2I
4(C
10H
8N
2)
3(C
3H
8O)
4]·2C
10H
8N
2}
n, (II), are one-dimensional polymers which are single- and double-stranded, respectively, the metal atoms being linked by the 4,4'-bipyridine moieties. The Mg complex, (I), is [
cis-{(H
2O)
4Mg(
N-4,4'-bipyridine-
N')
(2/2)}]
(|)I
2·4,4'-bipyridine and Mg has a six-coordinate quasi-octahedral coordination environment. The Sr complex, (II), is isomorphous with its previously defined Ba counterpart [Kepert, Waters & White (1996).
Aust. J. Chem. 49, 117-135], being [(propan-1-ol)
2I
2Sr(
N-4,4'-bipyridine-
N')
(3/2)]
(|)·4,4'-bipyridine, with the I atoms
trans-axial in a seven-coordinate pentagonal-bipyramidal Sr environment.
Supporting information
CCDC references: 226093; 226094
The complexes were obtained as outlined above. Analysis for (I): found: C 43.7, H 4.0, N 8.4%; C31H36I2N5O2Sr requires: C 43.70, H 4.26, N 8.22%. Analysis for (II): found: C 44.2, H 3.7, N 10.3%; C30H32I2MgN6O4 requires: C 44.01, H 3.94, N 10.26%.
The H atoms were located from difference Fourier maps and placed at idealized positions for those on C [C—H = 0.95 Å, UisoH = 1.25Ueq(C) (CH) and 1.5Ueq(C,O) (CH3 and OH)], and were refined (in x, y, z and U) for (I) but not refined for (II). Atoms C1A and C2A of one propanol group of (II) were each modelled as disordered over two sites, C1A and C1A', and C2A and C2A', and assigned site occupancy factors of 0.5 after initial trial refinement.
For both compounds, data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: Xtal3.5 (Hall et al., 1995); program(s) used to solve structure: Xtal3.5; program(s) used to refine structure: CRYLSQ in Xtal3.5; molecular graphics: Xtal3.5; software used to prepare material for publication: BONDLA and CIFIO in Xtal3.5.
(I)
catena-poly[[[tetraaquamagnesium(I)]-µ-4,4'-bipyridine-
κ2N:
N'] diiodide bis(4,4'-bipyridine) solvate]
top
Crystal data top
[Mg(C10H8N2)(H2O)4]I2·2C10H8N2 | F(000) = 1616 |
Mr = 818.75 | Dx = 1.577 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -c 2yc | Cell parameters from 8 reflections |
a = 27.574 (7) Å | θ = 18.1–23.8° |
b = 9.018 (4) Å | µ = 1.88 mm−1 |
c = 16.974 (3) Å | T = 298 K |
β = 125.23 (2)° | Block, colourless |
V = 3448 (2) Å3 | 0.35 × 0.33 × 0.32 mm |
Z = 4 | |
Data collection top
Enraf-Nonius CAD4 diffractometer | 2964 reflections with I > 2σ(I) |
Radiation source: sealed tube | Rint = 0.014 |
Graphite monochromator | θmax = 27.5°, θmin = 1.8° |
2θ/ω scans | h = −31→35 |
Absorption correction: gaussian (ABSORB in Xtal3.5; Hall et al., 1995) | k = −11→0 |
Tmin = 0.58, Tmax = 0.63 | l = −22→4 |
5196 measured reflections | 8 standard reflections every 60 min |
3955 independent reflections | intensity decay: none |
Refinement top
Refinement on F | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | All H-atom parameters refined |
wR(F2) = 0.052 | w = 1/[σ2(Fo)] where σ(I) = [σ(I)meas + 0.0004(Inet)2]1/2 |
S = 1.12 | (Δ/σ)max = 0.049 |
2964 reflections | Δρmax = 1.06 e Å−3 |
260 parameters | Δρmin = −0.50 e Å−3 |
0 restraints | Extinction correction: Zachariasen (1967), Eq. 22, p. 292
Larson, A. C. (1970). Crystallographic Computing, edited by F. R. Ahmed,
S. R. Hall & C. P. Huber, pp. 291-294. Copenhagen: Munksgaard. |
0 constraints | Extinction coefficient: 35 (4) × 103 |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
[Mg(C10H8N2)(H2O)4]I2·2C10H8N2 | V = 3448 (2) Å3 |
Mr = 818.75 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 27.574 (7) Å | µ = 1.88 mm−1 |
b = 9.018 (4) Å | T = 298 K |
c = 16.974 (3) Å | 0.35 × 0.33 × 0.32 mm |
β = 125.23 (2)° | |
Data collection top
Enraf-Nonius CAD4 diffractometer | 2964 reflections with I > 2σ(I) |
Absorption correction: gaussian (ABSORB in Xtal3.5; Hall et al., 1995) | Rint = 0.014 |
Tmin = 0.58, Tmax = 0.63 | 8 standard reflections every 60 min |
5196 measured reflections | intensity decay: none |
3955 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.040 | 0 restraints |
wR(F2) = 0.052 | All H-atom parameters refined |
S = 1.12 | Δρmax = 1.06 e Å−3 |
2964 reflections | Δρmin = −0.50 e Å−3 |
260 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
I | 0.348074 (13) | 0.25991 (3) | 0.18221 (2) | 0.0720 (2) | |
Mg | 0.50000 | 0.93393 (16) | 0.25000 | 0.0319 (6) | |
O1 | 0.50749 (14) | 1.0905 (3) | 0.1695 (2) | 0.0507 (12) | |
O2 | 0.59105 (11) | 0.9392 (3) | 0.33903 (19) | 0.0429 (12) | |
N11 | 0.50337 (14) | 0.7565 (3) | 0.3442 (2) | 0.0389 (13) | |
C12 | 0.54224 (17) | 0.7632 (4) | 0.4405 (3) | 0.0419 (16) | |
C13 | 0.54253 (16) | 0.6666 (4) | 0.5031 (2) | 0.0423 (16) | |
C14 | 0.50118 (15) | 0.5527 (4) | 0.4679 (2) | 0.0368 (14) | |
C15 | 0.46123 (19) | 0.5447 (4) | 0.3679 (3) | 0.0494 (15) | |
C16 | 0.46372 (18) | 0.6460 (4) | 0.3104 (3) | 0.0478 (15) | |
N21 | 0.81720 (15) | 0.6904 (5) | 0.4969 (3) | 0.0591 (17) | |
C22 | 0.79385 (19) | 0.8247 (6) | 0.4673 (3) | 0.0586 (18) | |
C23 | 0.74719 (17) | 0.8558 (5) | 0.3731 (3) | 0.0518 (16) | |
C24 | 0.72406 (16) | 0.7438 (4) | 0.3051 (3) | 0.0482 (16) | |
C25 | 0.7476 (2) | 0.6022 (5) | 0.3357 (3) | 0.0601 (15) | |
C26 | 0.7934 (2) | 0.5833 (6) | 0.4325 (3) | 0.066 (3) | |
N21' | 0.58234 (15) | 0.8219 (5) | 0.0100 (2) | 0.0577 (17) | |
C22' | 0.58681 (18) | 0.8943 (5) | 0.0811 (3) | 0.056 (2) | |
C23' | 0.63167 (17) | 0.8751 (5) | 0.1773 (3) | 0.051 (2) | |
C24' | 0.67539 (16) | 0.7715 (4) | 0.2026 (3) | 0.0465 (16) | |
C25' | 0.6709 (2) | 0.6945 (6) | 0.1287 (3) | 0.066 (3) | |
C26' | 0.6246 (2) | 0.7237 (6) | 0.0342 (4) | 0.072 (3) | |
H1A | 0.482 (2) | 1.128 (5) | 0.122 (3) | 0.061 (14)* | |
H1B | 0.533 (2) | 1.144 (5) | 0.194 (3) | 0.055 (14)* | |
H2A | 0.604 (2) | 1.009 (6) | 0.333 (3) | 0.074 (17)* | |
H2B | 0.619 (2) | 0.881 (5) | 0.384 (3) | 0.059 (12)* | |
H12 | 0.5701 (15) | 0.841 (4) | 0.462 (2) | 0.034 (9)* | |
H13 | 0.5711 (17) | 0.675 (5) | 0.571 (3) | 0.053 (11)* | |
H15 | 0.431 (2) | 0.474 (5) | 0.337 (3) | 0.062 (12)* | |
H16 | 0.4340 (19) | 0.647 (5) | 0.241 (3) | 0.069 (13)* | |
H22 | 0.8077 (18) | 0.899 (5) | 0.509 (3) | 0.056 (13)* | |
H23 | 0.7314 (15) | 0.957 (4) | 0.358 (3) | 0.040 (10)* | |
H25 | 0.7301 (16) | 0.519 (4) | 0.293 (3) | 0.047 (11)* | |
H26 | 0.8071 (18) | 0.490 (5) | 0.453 (3) | 0.065 (13)* | |
H22' | 0.5610 (18) | 0.968 (5) | 0.066 (3) | 0.055 (12)* | |
H23' | 0.6330 (17) | 0.932 (4) | 0.223 (3) | 0.046 (11)* | |
H25' | 0.699 (2) | 0.630 (6) | 0.138 (4) | 0.096 (18)* | |
H26' | 0.621 (2) | 0.666 (6) | −0.020 (4) | 0.086 (16)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I | 0.0525 (2) | 0.0580 (2) | 0.0736 (3) | 0.00823 (13) | 0.01793 (17) | −0.01955 (15) |
Mg | 0.0313 (7) | 0.0347 (8) | 0.0217 (7) | 0.00000 | 0.0106 (6) | 0.00000 |
O1 | 0.0409 (15) | 0.0555 (16) | 0.0314 (14) | −0.0050 (14) | 0.0068 (13) | 0.0153 (13) |
O2 | 0.0303 (12) | 0.0501 (15) | 0.0332 (14) | 0.0005 (11) | 0.0096 (11) | 0.0128 (12) |
N11 | 0.0441 (16) | 0.0393 (15) | 0.0311 (15) | −0.0025 (12) | 0.0205 (13) | 0.0020 (12) |
C12 | 0.0444 (19) | 0.046 (2) | 0.0322 (18) | −0.0106 (16) | 0.0203 (16) | −0.0028 (15) |
C13 | 0.0417 (19) | 0.049 (2) | 0.0251 (17) | −0.0075 (16) | 0.0129 (15) | −0.0006 (15) |
C14 | 0.0433 (18) | 0.0353 (16) | 0.0310 (17) | −0.0025 (14) | 0.0209 (15) | −0.0011 (13) |
C15 | 0.060 (2) | 0.046 (2) | 0.0312 (18) | −0.0175 (18) | 0.0200 (18) | −0.0053 (16) |
C16 | 0.055 (2) | 0.052 (2) | 0.0251 (17) | −0.0125 (18) | 0.0166 (17) | −0.0017 (16) |
N21 | 0.0374 (17) | 0.077 (2) | 0.042 (2) | 0.0060 (17) | 0.0109 (15) | 0.0200 (19) |
C22 | 0.043 (2) | 0.065 (3) | 0.047 (2) | −0.002 (2) | 0.014 (2) | 0.011 (2) |
C23 | 0.041 (2) | 0.058 (2) | 0.044 (2) | 0.0024 (18) | 0.0173 (18) | 0.012 (2) |
C24 | 0.0321 (17) | 0.061 (2) | 0.042 (2) | 0.0072 (16) | 0.0159 (16) | 0.0172 (18) |
C25 | 0.053 (2) | 0.058 (2) | 0.047 (2) | 0.011 (2) | 0.016 (2) | 0.010 (2) |
C26 | 0.053 (3) | 0.067 (3) | 0.053 (3) | 0.019 (2) | 0.016 (2) | 0.023 (2) |
N21' | 0.046 (2) | 0.079 (2) | 0.0324 (17) | 0.0043 (18) | 0.0136 (15) | 0.0157 (17) |
C22' | 0.040 (2) | 0.071 (3) | 0.044 (2) | 0.013 (2) | 0.0165 (18) | 0.023 (2) |
C23' | 0.042 (2) | 0.066 (3) | 0.040 (2) | 0.0130 (18) | 0.0211 (18) | 0.014 (2) |
C24' | 0.0358 (18) | 0.060 (2) | 0.038 (2) | 0.0088 (16) | 0.0180 (16) | 0.0145 (17) |
C25' | 0.056 (3) | 0.082 (3) | 0.048 (3) | 0.025 (2) | 0.023 (2) | 0.007 (2) |
C26' | 0.068 (3) | 0.090 (4) | 0.042 (2) | 0.009 (3) | 0.022 (2) | 0.007 (2) |
Geometric parameters (Å, º) top
Mg—O1 | 2.056 (4) | N21—C22 | 1.327 (7) |
Mg—O2 | 2.052 (3) | N21—C26 | 1.316 (6) |
Mg—N11 | 2.226 (4) | C22—C23 | 1.385 (5) |
Mg—O1 | 2.056 (4) | C22—H22 | 0.89 (4) |
Mg—O2 | 2.052 (3) | C23—C24 | 1.382 (6) |
Mg—N11 | 2.226 (4) | C23—H23 | 0.98 (4) |
O1—H1A | 0.78 (4) | C24—C25 | 1.390 (6) |
O1—H1B | 0.75 (4) | C24—C24' | 1.482 (5) |
O2—H2A | 0.76 (6) | C25—C26 | 1.389 (5) |
O2—H2B | 0.88 (4) | C25—H25 | 0.96 (4) |
N11—C12 | 1.343 (5) | C26—H26 | 0.91 (4) |
N11—C16 | 1.339 (5) | N21'—C22' | 1.314 (7) |
C12—C13 | 1.370 (6) | N21'—C26' | 1.326 (7) |
C12—H12 | 0.94 (4) | C22'—C23' | 1.377 (5) |
C13—C14 | 1.388 (5) | C22'—H22' | 0.90 (5) |
C13—H13 | 0.95 (4) | C23'—C24' | 1.383 (6) |
C14—C15 | 1.394 (5) | C23'—H23' | 0.91 (5) |
C14—C14 | 1.475 (6) | C24'—C25' | 1.375 (8) |
C15—C16 | 1.367 (7) | C25'—C26' | 1.382 (6) |
C15—H15 | 0.93 (4) | C25'—H25' | 0.91 (6) |
C16—H16 | 0.97 (4) | C26'—H26' | 1.01 (7) |
| | | |
O1—Mg—O2 | 85.66 (12) | N11—C16—C15 | 123.8 (3) |
O1—Mg—N11 | 172.90 (14) | N11—C16—H16 | 115 (3) |
O1—Mg—O1 | 93.28 (15) | C15—C16—H16 | 121 (3) |
O1—Mg—O2 | 92.52 (13) | C22—N21—C26 | 117.1 (4) |
O1—Mg—N11 | 89.70 (13) | N21—C22—C23 | 123.1 (4) |
O2—Mg—N11 | 87.78 (12) | N21—C22—H22 | 120 (3) |
O2—Mg—O1 | 92.52 (13) | C23—C22—H22 | 117 (3) |
O2—Mg—O2 | 177.35 (14) | C22—C23—C24 | 119.4 (4) |
O2—Mg—N11 | 94.13 (13) | C22—C23—H23 | 118 (2) |
N11—Mg—O1 | 89.70 (13) | C24—C23—H23 | 123 (2) |
N11—Mg—O2 | 94.13 (13) | C23—C24—C25 | 117.9 (3) |
N11—Mg—N11 | 88.08 (14) | C23—C24—C24' | 121.8 (3) |
O1—Mg—O2 | 85.66 (13) | C25—C24—C24' | 120.3 (3) |
O1—Mg—N11 | 172.90 (14) | C24—C25—C26 | 117.7 (4) |
O2—Mg—N11 | 87.78 (12) | C24—C25—H25 | 121 (2) |
Mg—O1—H1A | 128 (4) | C26—C25—H25 | 121 (2) |
Mg—O1—H1B | 120 (4) | N21—C26—C25 | 124.8 (5) |
H1A—O1—H1B | 107 (5) | N21—C26—H26 | 118 (2) |
Mg—O2—H2A | 113 (3) | C25—C26—H26 | 117 (2) |
Mg—O2—H2B | 135 (3) | C22'—N21'—C26' | 116.6 (4) |
H2A—O2—H2B | 112 (5) | N21'—C22'—C23' | 124.8 (4) |
Mg—N11—C12 | 121.0 (3) | N21'—C22'—H22' | 118 (3) |
Mg—N11—C16 | 122.8 (2) | C23'—C22'—H22' | 117 (3) |
C12—N11—C16 | 115.9 (4) | C22'—C23'—C24' | 118.6 (5) |
N11—C12—C13 | 124.0 (3) | C22'—C23'—H23' | 120 (2) |
N11—C12—H12 | 114 (2) | C24'—C23'—H23' | 121 (2) |
C13—C12—H12 | 122 (2) | C24—C24'—C23' | 121.0 (5) |
C12—C13—C14 | 120.1 (3) | C24—C24'—C25' | 122.0 (4) |
C12—C13—H13 | 121 (3) | C23'—C24'—C25' | 117.0 (4) |
C14—C13—H13 | 119 (3) | C24'—C25'—C26' | 120.0 (5) |
C13—C14—C15 | 116.0 (4) | C24'—C25'—H25' | 123 (4) |
C13—C14—C14 | 122.3 (3) | C26'—C25'—H25' | 117 (4) |
C15—C14—C14 | 121.7 (3) | N21'—C26'—C25' | 123.0 (6) |
C14—C15—C16 | 120.3 (4) | N21'—C26'—H26' | 117 (2) |
C14—C15—H15 | 123 (3) | C25'—C26'—H26' | 120 (3) |
C16—C15—H15 | 117 (3) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1B···Ii | 0.76 (5) | 2.88 (4) | 3.601 (3) | 161 (4) |
O2—H2A···Ii | 0.75 (6) | 2.71 (6) | 3.466 (3) | 178 (5) |
Symmetry code: (i) −x+1, y+1, −z+1/2. |
(II)
catena-poly[[[[µ-4,4'-bipyridine-bis[diiodobis(propan-1-ol)strontium(I)]]- di-µ-4,4'-bipyridine-
κ4N:
N'] bis(4,4'-bipyridine) solvate] [Sr
2I
4(C
10H
8N
2)
3(C
3H
8O)
4]·2C
10H
8N
2 top
Crystal data top
[Sr2I4(C10H8N2)3(C3H8O)4]·2C10H8N2 | F(000) = 1668 |
Mr = 1704.2 | Dx = 1.612 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -p 2ybc | Cell parameters from 8 reflections |
a = 15.365 (2) Å | θ = 16.7–18.5° |
b = 12.392 (2) Å | µ = 3.33 mm−1 |
c = 20.979 (2) Å | T = 298 K |
β = 118.493 (8)° | Prism, colourless |
V = 3510.6 (8) Å3 | 0.53 × 0.40 × 0.18 mm |
Z = 2 | |
Data collection top
Enraf-Nonius CAD4 with CCD area-detector diffractometer | 6161 independent reflections |
Radiation source: sealed tube | 4203 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
2θ/ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: gaussian (ABSORB in Xtal3.5; Hall et al., 1995) | h = −18→18 |
Tmin = 0.33, Tmax = 0.56 | k = −14→0 |
11868 measured reflections | l = −24→21 |
Refinement top
Refinement on F | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.044 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.05 | H-atom parameters constrained |
S = 1.16 | w = 1/[σ2(Fo)] where σ(I) = [σ(I)meas + 0.0004(Inet)2]1/2 |
4203 reflections | (Δ/σ)max = 0.005 |
388 parameters | Δρmax = 0.87 e Å−3 |
0 restraints | Δρmin = −0.55 e Å−3 |
0 constraints | |
Crystal data top
[Sr2I4(C10H8N2)3(C3H8O)4]·2C10H8N2 | V = 3510.6 (8) Å3 |
Mr = 1704.2 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 15.365 (2) Å | µ = 3.33 mm−1 |
b = 12.392 (2) Å | T = 298 K |
c = 20.979 (2) Å | 0.53 × 0.40 × 0.18 mm |
β = 118.493 (8)° | |
Data collection top
Enraf-Nonius CAD4 with CCD area-detector diffractometer | 6161 independent reflections |
Absorption correction: gaussian (ABSORB in Xtal3.5; Hall et al., 1995) | 4203 reflections with I > 2σ(I) |
Tmin = 0.33, Tmax = 0.56 | Rint = 0.025 |
11868 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.044 | 0 restraints |
wR(F2) = 0.05 | H-atom parameters constrained |
S = 1.16 | Δρmax = 0.87 e Å−3 |
4203 reflections | Δρmin = −0.55 e Å−3 |
388 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sr | 0.25574 (4) | 0.71094 (4) | 0.22114 (3) | 0.0322 (3) | |
I1 | 0.08983 (4) | 0.70739 (4) | 0.27557 (3) | 0.0572 (3) | |
I2 | 0.43301 (4) | 0.72360 (4) | 0.17645 (3) | 0.0670 (3) | |
O1A | 0.3664 (4) | 0.5844 (4) | 0.3238 (3) | 0.063 (3) | |
C1A | 0.4693 (15) | 0.5601 (17) | 0.3459 (9) | 0.050 (9) | 0.50000 |
C1A' | 0.466 (2) | 0.592 (2) | 0.386 (3) | 0.12 (2) | 0.50000 |
C2A | 0.516 (2) | 0.545 (2) | 0.4318 (10) | 0.065 (11) | 0.50000 |
C2A' | 0.5318 (18) | 0.521 (2) | 0.397 (2) | 0.117 (18) | 0.50000 |
C3A | 0.6272 (8) | 0.5221 (12) | 0.4597 (6) | 0.136 (9) | |
O1B | 0.1329 (4) | 0.7077 (4) | 0.0833 (3) | 0.065 (3) | |
C1B | 0.0794 (8) | 0.7947 (8) | 0.0349 (6) | 0.098 (6) | |
C2B | 0.1317 (11) | 0.8404 (9) | −0.0006 (6) | 0.130 (9) | |
C3B | 0.0923 (9) | 0.9478 (10) | −0.0357 (6) | 0.130 (8) | |
N11 | 0.2080 (4) | 0.5016 (4) | 0.1783 (3) | 0.052 (3) | |
C12 | 0.2825 (6) | 0.4417 (5) | 0.1812 (4) | 0.060 (4) | |
C13 | 0.2852 (5) | 0.3317 (5) | 0.1831 (4) | 0.056 (4) | |
C14 | 0.2060 (5) | 0.2747 (5) | 0.1799 (4) | 0.044 (3) | |
C15 | 0.1254 (5) | 0.3348 (5) | 0.1741 (4) | 0.048 (3) | |
C16 | 0.1308 (5) | 0.4468 (5) | 0.1742 (4) | 0.049 (4) | |
N11' | 0.2155 (5) | −0.0713 (4) | 0.1952 (3) | 0.054 (3) | |
C12' | 0.2691 (6) | −0.0164 (6) | 0.1724 (5) | 0.065 (4) | |
C13' | 0.2678 (6) | 0.0945 (5) | 0.1667 (4) | 0.061 (4) | |
C14' | 0.2064 (5) | 0.1550 (5) | 0.1844 (4) | 0.044 (3) | |
C15' | 0.1513 (5) | 0.0981 (5) | 0.2080 (4) | 0.056 (4) | |
C16' | 0.1560 (5) | −0.0134 (5) | 0.2124 (4) | 0.054 (4) | |
N21 | 0.3767 (5) | 0.8314 (5) | 0.3449 (3) | 0.061 (3) | |
C22 | 0.4382 (7) | 0.9094 (7) | 0.3487 (4) | 0.078 (5) | |
C23 | 0.4865 (6) | 0.9767 (6) | 0.4074 (4) | 0.068 (5) | |
C24 | 0.4752 (5) | 0.9636 (5) | 0.4676 (4) | 0.050 (4) | |
C25 | 0.4137 (6) | 0.8801 (6) | 0.4655 (4) | 0.065 (4) | |
C26 | 0.3681 (6) | 0.8175 (6) | 0.4046 (4) | 0.069 (5) | |
N31 | −0.2884 (5) | 0.8975 (5) | 0.1497 (3) | 0.060 (3) | |
C32 | −0.2033 (6) | 0.9039 (6) | 0.1471 (4) | 0.059 (4) | |
C33 | −0.1659 (5) | 0.8204 (6) | 0.1243 (4) | 0.051 (4) | |
C34 | −0.2161 (5) | 0.7234 (5) | 0.1022 (4) | 0.050 (4) | |
C35 | −0.3019 (6) | 0.7164 (5) | 0.1077 (5) | 0.066 (4) | |
C36 | −0.3354 (6) | 0.8037 (7) | 0.1310 (5) | 0.067 (5) | |
N31' | −0.1235 (5) | 0.4614 (5) | 0.0145 (4) | 0.072 (4) | |
C32' | −0.1065 (7) | 0.5611 (7) | 0.0077 (5) | 0.080 (6) | |
C33' | −0.1337 (7) | 0.6479 (6) | 0.0358 (5) | 0.074 (5) | |
C34' | −0.1815 (5) | 0.6332 (6) | 0.0748 (4) | 0.052 (4) | |
C35' | −0.1941 (8) | 0.5261 (7) | 0.0882 (6) | 0.097 (6) | |
C36' | −0.1624 (9) | 0.4454 (7) | 0.0574 (6) | 0.102 (7) | |
H1OA | 0.32536 | 0.52518 | 0.31657 | 0.07300* | |
H1AA | 0.50145 | 0.62076 | 0.33515 | 0.05600* | 0.50000 |
H1AB | 0.47739 | 0.49859 | 0.32214 | 0.05600* | 0.50000 |
H2AA | 0.48432 | 0.48343 | 0.44326 | 0.07300* | 0.50000 |
H2AB | 0.50619 | 0.60602 | 0.45609 | 0.07300* | 0.50000 |
H3AA | 0.65643 | 0.51010 | 0.50986 | 0.18200* | 0.50000 |
H3AB | 0.65157 | 0.58238 | 0.44786 | 0.18200* | 0.50000 |
H3AC | 0.62970 | 0.45979 | 0.43503 | 0.18200* | 0.50000 |
H1A'A | 0.46363 | 0.59164 | 0.43272 | 0.13700* | 0.50000 |
H1A'B | 0.49959 | 0.65847 | 0.38719 | 0.13700* | 0.50000 |
H2A'A | 0.54456 | 0.52502 | 0.35513 | 0.14500* | 0.50000 |
H2A'B | 0.50408 | 0.45037 | 0.39433 | 0.14500* | 0.50000 |
H3A'A | 0.66288 | 0.46263 | 0.45954 | 0.18200* | 0.50000 |
H3A'B | 0.61453 | 0.51915 | 0.50082 | 0.18200* | 0.50000 |
H3A'C | 0.65535 | 0.58750 | 0.45898 | 0.18200* | 0.50000 |
H1OB | 0.16484 | 0.68247 | 0.05808 | 0.08000* | |
H1BA | 0.06952 | 0.84974 | 0.06218 | 0.11400* | |
H1BB | 0.01790 | 0.76810 | −0.00100 | 0.11400* | |
H2BA | 0.12891 | 0.79051 | −0.03600 | 0.13900* | |
H2BB | 0.20040 | 0.84893 | 0.03545 | 0.13900* | |
H3BA | 0.12968 | 0.97330 | −0.05756 | 0.15300* | |
H3BB | 0.09648 | 0.99766 | 0.00015 | 0.15300* | |
H3BC | 0.02499 | 0.93924 | −0.07130 | 0.15300* | |
H12 | 0.33815 | 0.47837 | 0.18209 | 0.07500* | |
H13 | 0.34166 | 0.29400 | 0.18659 | 0.06700* | |
H15 | 0.06798 | 0.29941 | 0.16994 | 0.05900* | |
H16 | 0.07653 | 0.48689 | 0.17138 | 0.05900* | |
H12' | 0.31127 | −0.05595 | 0.15889 | 0.07600* | |
H13' | 0.30960 | 0.12961 | 0.15116 | 0.07200* | |
H15' | 0.10953 | 0.13604 | 0.22225 | 0.06700* | |
H16' | 0.11575 | −0.05028 | 0.22867 | 0.06100* | |
H22 | 0.45022 | 0.91893 | 0.30871 | 0.09200* | |
H23 | 0.52834 | 1.03311 | 0.40642 | 0.08000* | |
H25 | 0.40294 | 0.86722 | 0.50608 | 0.07500* | |
H26 | 0.32693 | 0.75999 | 0.40458 | 0.09100* | |
H32 | −0.16758 | 0.96930 | 0.16181 | 0.06800* | |
H33 | −0.10515 | 0.82864 | 0.12379 | 0.06400* | |
H35 | −0.33902 | 0.65051 | 0.09537 | 0.07600* | |
H36 | −0.39581 | 0.79613 | 0.13349 | 0.08200* | |
H32' | −0.07265 | 0.57670 | −0.01914 | 0.09600* | |
H33' | −0.11907 | 0.71944 | 0.02730 | 0.09100* | |
H35' | −0.22291 | 0.50853 | 0.11867 | 0.11500* | |
H36' | −0.17239 | 0.37279 | 0.06747 | 0.11800* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sr | 0.0416 (3) | 0.0160 (3) | 0.0442 (3) | −0.0020 (2) | 0.0246 (3) | −0.0019 (2) |
I1 | 0.0597 (3) | 0.0462 (3) | 0.0834 (4) | 0.0015 (2) | 0.0484 (3) | 0.0033 (3) |
I2 | 0.0749 (4) | 0.0499 (3) | 0.1055 (5) | −0.0035 (3) | 0.0666 (4) | −0.0065 (3) |
O1A | 0.058 (3) | 0.044 (3) | 0.075 (4) | −0.005 (2) | 0.023 (3) | 0.012 (3) |
C1A | 0.031 (10) | 0.068 (12) | 0.042 (11) | 0.001 (8) | 0.011 (9) | 0.005 (9) |
C1A' | 0.10 (2) | 0.11 (2) | 0.13 (3) | 0.032 (17) | 0.05 (2) | 0.03 (2) |
C2A | 0.084 (16) | 0.076 (13) | 0.047 (12) | 0.022 (11) | 0.042 (12) | 0.001 (10) |
C2A' | 0.057 (16) | 0.15 (2) | 0.13 (3) | 0.007 (15) | 0.04 (2) | −0.03 (2) |
C3A | 0.081 (8) | 0.227 (15) | 0.088 (8) | 0.031 (9) | 0.029 (7) | −0.020 (9) |
O1B | 0.092 (4) | 0.043 (3) | 0.062 (3) | 0.012 (3) | 0.038 (3) | 0.000 (3) |
C1B | 0.130 (9) | 0.069 (6) | 0.084 (7) | −0.008 (6) | 0.042 (7) | −0.009 (6) |
C2B | 0.225 (14) | 0.072 (7) | 0.111 (9) | −0.022 (8) | 0.096 (10) | −0.014 (7) |
C3B | 0.158 (11) | 0.099 (9) | 0.123 (10) | −0.004 (8) | 0.059 (9) | 0.031 (7) |
N11 | 0.066 (4) | 0.025 (3) | 0.067 (4) | 0.002 (3) | 0.033 (3) | −0.002 (3) |
C12 | 0.070 (5) | 0.033 (4) | 0.089 (6) | −0.007 (4) | 0.049 (5) | −0.001 (4) |
C13 | 0.065 (5) | 0.025 (3) | 0.091 (6) | 0.003 (3) | 0.046 (5) | −0.002 (4) |
C14 | 0.052 (4) | 0.023 (3) | 0.057 (4) | −0.006 (3) | 0.026 (4) | −0.002 (3) |
C15 | 0.053 (4) | 0.024 (3) | 0.064 (5) | −0.008 (3) | 0.027 (4) | −0.008 (3) |
C16 | 0.057 (5) | 0.032 (4) | 0.059 (5) | 0.004 (3) | 0.028 (4) | −0.004 (3) |
N11' | 0.071 (4) | 0.027 (3) | 0.065 (4) | 0.001 (3) | 0.035 (3) | −0.004 (3) |
C12' | 0.083 (6) | 0.034 (4) | 0.099 (6) | 0.002 (4) | 0.061 (5) | −0.006 (4) |
C13' | 0.084 (6) | 0.029 (4) | 0.093 (6) | 0.001 (4) | 0.060 (5) | −0.001 (4) |
C14' | 0.051 (4) | 0.028 (3) | 0.053 (4) | −0.000 (3) | 0.025 (4) | −0.002 (3) |
C15' | 0.067 (5) | 0.030 (4) | 0.082 (6) | −0.002 (3) | 0.046 (4) | −0.004 (4) |
C16' | 0.071 (5) | 0.028 (4) | 0.076 (5) | −0.010 (3) | 0.045 (4) | −0.000 (3) |
N21 | 0.076 (4) | 0.046 (4) | 0.052 (4) | −0.012 (3) | 0.024 (3) | −0.006 (3) |
C22 | 0.122 (8) | 0.062 (5) | 0.057 (5) | −0.035 (5) | 0.047 (5) | −0.008 (4) |
C23 | 0.093 (6) | 0.051 (5) | 0.063 (5) | −0.029 (4) | 0.039 (5) | −0.006 (4) |
C24 | 0.050 (4) | 0.038 (4) | 0.054 (5) | −0.004 (3) | 0.019 (4) | 0.002 (3) |
C25 | 0.079 (6) | 0.059 (5) | 0.060 (5) | −0.031 (4) | 0.035 (4) | −0.022 (4) |
C26 | 0.085 (6) | 0.057 (5) | 0.067 (6) | −0.031 (4) | 0.038 (5) | −0.016 (4) |
N31 | 0.067 (4) | 0.048 (4) | 0.072 (4) | −0.002 (3) | 0.039 (4) | −0.015 (3) |
C32 | 0.072 (5) | 0.045 (4) | 0.062 (5) | −0.006 (4) | 0.033 (4) | −0.012 (4) |
C33 | 0.055 (4) | 0.043 (4) | 0.062 (5) | −0.003 (3) | 0.033 (4) | −0.009 (3) |
C34 | 0.056 (4) | 0.037 (4) | 0.067 (5) | −0.001 (3) | 0.036 (4) | −0.004 (3) |
C35 | 0.083 (6) | 0.035 (4) | 0.091 (6) | −0.010 (4) | 0.051 (5) | −0.018 (4) |
C36 | 0.069 (5) | 0.064 (5) | 0.087 (6) | −0.010 (4) | 0.053 (5) | −0.018 (5) |
N31' | 0.099 (5) | 0.047 (4) | 0.097 (5) | −0.006 (4) | 0.069 (5) | −0.014 (4) |
C32' | 0.113 (7) | 0.062 (6) | 0.100 (7) | −0.006 (5) | 0.080 (6) | −0.015 (5) |
C33' | 0.106 (7) | 0.047 (5) | 0.093 (6) | −0.011 (5) | 0.068 (6) | −0.012 (4) |
C34' | 0.064 (5) | 0.045 (4) | 0.062 (5) | −0.010 (4) | 0.041 (4) | −0.010 (4) |
C35' | 0.155 (9) | 0.049 (5) | 0.147 (9) | 0.004 (6) | 0.120 (8) | 0.002 (5) |
C36' | 0.163 (10) | 0.046 (5) | 0.150 (10) | 0.003 (6) | 0.117 (9) | −0.001 (6) |
Geometric parameters (Å, º) top
Sr—I1 | 3.2530 (11) | C14—C14' | 1.485 (8) |
Sr—I2 | 3.2801 (11) | C15—C16 | 1.389 (9) |
Sr—O1A | 2.549 (4) | C15—H15 | 0.952 |
Sr—O1B | 2.592 (4) | C16—H16 | 0.948 |
Sr—N11 | 2.729 (5) | N11'—C12' | 1.321 (13) |
Sr—N21 | 2.797 (5) | N11'—C16' | 1.339 (12) |
Sr—N11' | 2.764 (5) | C12'—C13' | 1.378 (10) |
O1A—C1A | 1.45 (2) | C12'—H12' | 0.958 |
O1A—C1A' | 1.46 (3) | C13'—C14' | 1.388 (13) |
O1A—H1OA | 0.931 | C13'—H13' | 0.953 |
C1A—C2A | 1.60 (3) | C14'—C15' | 1.364 (13) |
C1A—H1AA | 0.98 | C15'—C16' | 1.385 (9) |
C1A—H1AB | 0.95 | C15'—H15' | 0.951 |
C1A'—C2A' | 1.28 (5) | C16'—H16' | 0.954 |
C1A'—H1A'A | 0.99 | N21—C22 | 1.328 (12) |
C1A'—H1A'B | 0.97 | N21—C26 | 1.331 (13) |
C2A—C3A | 1.55 (3) | C22—C23 | 1.375 (11) |
C2A—H2AA | 1.00 | C22—H22 | 0.949 |
C2A—H2AB | 0.96 | C23—C24 | 1.363 (14) |
C2A'—C3A | 1.43 (3) | C23—H23 | 0.956 |
C2A'—H2A'A | 0.98 | C24—C25 | 1.388 (11) |
C2A'—H2A'B | 0.96 | C24—C24 | 1.503 (9) |
C3A—H3AA | 0.938 | C25—C26 | 1.369 (11) |
C3A—H3AB | 0.922 | C25—H25 | 0.955 |
C3A—H3AC | 0.941 | C26—H26 | 0.953 |
C3A—H3A'A | 0.920 | N31—C32 | 1.336 (13) |
C3A—H3A'B | 0.970 | N31—C36 | 1.324 (10) |
C3A—H3A'C | 0.922 | C32—C33 | 1.376 (12) |
O1B—C1B | 1.440 (10) | C32—H32 | 0.945 |
O1B—H1OB | 0.930 | C33—C34 | 1.384 (9) |
C1B—C2B | 1.45 (2) | C33—H33 | 0.944 |
C1B—H1BA | 0.948 | C34—C35 | 1.380 (14) |
C1B—H1BB | 0.943 | C34—C34' | 1.467 (11) |
C2B—C3B | 1.501 (16) | C35—C36 | 1.383 (13) |
C2B—H2BA | 0.951 | C35—H35 | 0.958 |
C2B—H2BB | 0.967 | C36—H36 | 0.959 |
C3B—H3BA | 0.945 | N31'—C32' | 1.286 (11) |
C3B—H3BB | 0.952 | N31'—C36' | 1.311 (18) |
C3B—H3BC | 0.949 | C32'—C33' | 1.384 (14) |
N11—C12 | 1.341 (11) | C32'—H32' | 0.950 |
N11—C16 | 1.333 (10) | C33'—C34' | 1.348 (16) |
C12—C13 | 1.364 (9) | C33'—H33' | 0.952 |
C12—H12 | 0.961 | C34'—C35' | 1.390 (12) |
C13—C14 | 1.381 (11) | C35'—C36' | 1.398 (17) |
C13—H13 | 0.958 | C35'—H35' | 0.960 |
C14—C15 | 1.399 (11) | C36'—H36' | 0.954 |
| | | |
I1—Sr—I2 | 176.07 (2) | N11—C12—C13 | 124.5 (8) |
I1—Sr—O1A | 90.77 (16) | N11—C12—H12 | 118.2 |
I1—Sr—O1B | 96.68 (16) | C13—C12—H12 | 117.3 |
I1—Sr—N11 | 88.27 (17) | C12—C13—C14 | 119.8 (8) |
I1—Sr—N21 | 88.06 (17) | C12—C13—H13 | 120.2 |
I1—Sr—N11' | 86.74 (17) | C14—C13—H13 | 120.0 |
I2—Sr—O1A | 87.76 (15) | C13—C14—C15 | 117.0 (6) |
I2—Sr—O1B | 86.76 (16) | C13—C14—C14' | 122.0 (7) |
I2—Sr—N11 | 94.66 (17) | C15—C14—C14' | 121.0 (7) |
I2—Sr—N21 | 88.01 (17) | C14—C15—C16 | 118.8 (7) |
I2—Sr—N11' | 92.03 (17) | C14—C15—H15 | 120.3 |
O1A—Sr—O1B | 140.38 (15) | C16—C15—H15 | 120.8 |
O1A—Sr—N11 | 70.08 (15) | N11—C16—C15 | 124.0 (7) |
O1A—Sr—N21 | 70.34 (16) | N11—C16—H16 | 117.7 |
O1A—Sr—N11' | 139.79 (15) | C15—C16—H16 | 118.3 |
O1B—Sr—N11 | 71.32 (15) | C12'—N11'—C16' | 116.4 (6) |
O1B—Sr—N21 | 148.43 (16) | C12'—N11'—Sr | 117.0 (5) |
O1B—Sr—N11' | 79.64 (15) | C16'—N11'—Sr | 126.0 (5) |
N11—Sr—N21 | 140.18 (16) | N11'—C12'—C13' | 124.0 (9) |
N11—Sr—N11' | 149.72 (15) | N11'—C12'—H12' | 118.1 |
N21—Sr—N11' | 69.46 (16) | C13'—C12'—H12' | 117.9 |
Sr—O1A—C1A | 125.7 (9) | C12'—C13'—C14' | 119.9 (9) |
Sr—O1A—C1A' | 135.0 (14) | C12'—C13'—H13' | 120.1 |
Sr—O1A—H1OA | 102.7 | C14'—C13'—H13' | 120.0 |
C1A—O1A—H1OA | 116.0 | C14—C14'—C13' | 120.4 (8) |
C1A'—O1A—H1OA | 122.1 | C14—C14'—C15' | 123.7 (8) |
O1A—C1A—C2A | 102.6 (19) | C13'—C14'—C15' | 115.9 (6) |
O1A—C1A—H1AA | 111.0 | C14'—C15'—C16' | 121.2 (9) |
O1A—C1A—H1AB | 113.2 | C14'—C15'—H15' | 119.2 |
C2A—C1A—H1AA | 110.0 | C16'—C15'—H15' | 119.6 |
C2A—C1A—H1AB | 113.3 | N11'—C16'—C15' | 122.6 (9) |
H1AA—C1A—H1AB | 107 | N11'—C16'—H16' | 118.8 |
O1A—C1A'—C2A' | 121 (3) | C15'—C16'—H16' | 118.6 |
O1A—C1A'—H1A'A | 112 | Sr—N21—C22 | 125.7 (6) |
O1A—C1A'—H1A'B | 113 | Sr—N21—C26 | 119.0 (5) |
C2A'—C1A'—H1A'A | 103 | C22—N21—C26 | 115.2 (7) |
C2A'—C1A'—H1A'B | 102 | N21—C22—C23 | 124.1 (10) |
H1A'A—C1A'—H1A'B | 104 | N21—C22—H22 | 118.1 |
C1A—C2A—C3A | 106 (2) | C23—C22—H22 | 117.9 |
C1A—C2A—H2AA | 110.7 | C22—C23—C24 | 120.3 (8) |
C1A—C2A—H2AB | 114.0 | C22—C23—H23 | 120.3 |
C3A—C2A—H2AA | 110.2 | C24—C23—H23 | 119.4 |
C3A—C2A—H2AB | 111.6 | C23—C24—C25 | 116.5 (7) |
H2AA—C2A—H2AB | 105 | C23—C24—C24 | 122.2 (7) |
C1A'—C2A'—H2A'A | 107 | C25—C24—C24 | 121.3 (8) |
C1A'—C2A'—H2A'B | 108 | C24—C25—C26 | 119.3 (9) |
H2A'A—C2A'—H2A'B | 106 | C24—C25—H25 | 120.2 |
C2A—C3A—H3AA | 107.9 | C26—C25—H25 | 120.6 |
C2A—C3A—H3AB | 105.5 | N21—C26—C25 | 124.7 (8) |
C2A—C3A—H3AC | 105.7 | N21—C26—H26 | 117.4 |
C2A'—C3A—H3A'A | 109.7 | C25—C26—H26 | 117.9 |
C2A'—C3A—H3A'B | 106 | C32—N31—C36 | 116.5 (8) |
C2A'—C3A—H3A'C | 106.0 | N31—C32—C33 | 123.3 (7) |
H3AA—C3A—H3AB | 11313 | N31—C32—H32 | 117.8 |
H3AA—C3A—H3AC | 111.3 | C33—C32—H32 | 118.9 |
H3AB—C3A—H3AC | 112.8 | C32—C33—C34 | 120.7 (8) |
H3A'A—C3A—H3A'B | 110.2 | C32—C33—H33 | 120.2 |
H3A'A—C3A—H3A'C | 114.7 | C34—C33—H33 | 119.1 |
H3A'B—C3A—H3A'C | 110.1 | C33—C34—C35 | 115.4 (7) |
Sr—O1B—C1B | 129.9 (5) | C33—C34—C34' | 123.0 (8) |
Sr—O1B—H1OB | 109.8 | C35—C34—C34' | 121.6 (6) |
C1B—O1B—H1OB | 97.4 | C34—C35—C36 | 120.7 (7) |
O1B—C1B—C2B | 112.7 (10) | C34—C35—H35 | 119.9 |
O1B—C1B—H1BA | 108.3 | C36—C35—H35 | 119.3 |
O1B—C1B—H1BB | 108.6 | N31—C36—C35 | 123.3 (9) |
C2B—C1B—H1BA | 108.5 | N31—C36—H36 | 118.4 |
C2B—C1B—H1BB | 108.5 | C35—C36—H36 | 118.3 |
H1BA—C1B—H1BB | 110.2 | C32'—N31'—C36' | 113.9 (9) |
C1B—C2B—C3B | 113.9 (13) | N31'—C32'—C33' | 125.5 (12) |
C1B—C2B—H2BA | 108.5 | N31'—C32'—H32' | 117.3 |
C1B—C2B—H2BB | 107.8 | C33'—C32'—H32' | 117.2 |
C3B—C2B—H2BA | 109.7 | C32'—C33'—C34' | 121.1 (8) |
C3B—C2B—H2BB | 108.8 | C32'—C33'—H33' | 119.8 |
H2BA—C2B—H2BB | 108.0 | C34'—C33'—H33' | 119.1 |
C2B—C3B—H3BA | 109.7 | C34—C34'—C33' | 122.7 (7) |
C2B—C3B—H3BB | 109.2 | C34—C34'—C35' | 122.5 (10) |
C2B—C3B—H3BC | 108.7 | C33'—C34'—C35' | 114.9 (9) |
H3BA—C3B—H3BB | 109.8 | C34'—C35'—C36' | 118.5 (12) |
H3BA—C3B—H3BC | 110.0 | C34'—C35'—H35' | 120.3 |
H3BB—C3B—H3BC | 109.4 | C36'—C35'—H35' | 121.2 |
Sr—N11—C12 | 114.9 (4) | N31'—C36'—C35' | 125.7 (9) |
Sr—N11—C16 | 126.7 (5) | N31'—C36'—H36' | 117.9 |
C12—N11—C16 | 115.8 (6) | C35'—C36'—H36' | 116.4 |
Experimental details
| (I) | (II) |
Crystal data |
Chemical formula | [Mg(C10H8N2)(H2O)4]I2·2C10H8N2 | [Sr2I4(C10H8N2)3(C3H8O)4]·2C10H8N2 |
Mr | 818.75 | 1704.2 |
Crystal system, space group | Monoclinic, C2/c | Monoclinic, P21/c |
Temperature (K) | 298 | 298 |
a, b, c (Å) | 27.574 (7), 9.018 (4), 16.974 (3) | 15.365 (2), 12.392 (2), 20.979 (2) |
β (°) | 125.23 (2) | 118.493 (8) |
V (Å3) | 3448 (2) | 3510.6 (8) |
Z | 4 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 1.88 | 3.33 |
Crystal size (mm) | 0.35 × 0.33 × 0.32 | 0.53 × 0.40 × 0.18 |
|
Data collection |
Diffractometer | Enraf-Nonius CAD4 diffractometer | Enraf-Nonius CAD4 with CCD area-detector diffractometer |
Absorption correction | Gaussian (ABSORB in Xtal3.5; Hall et al., 1995) | Gaussian (ABSORB in Xtal3.5; Hall et al., 1995) |
Tmin, Tmax | 0.58, 0.63 | 0.33, 0.56 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5196, 3955, 2964 | 11868, 6161, 4203 |
Rint | 0.014 | 0.025 |
(sin θ/λ)max (Å−1) | 0.650 | 0.595 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.040, 0.052, 1.12 | 0.044, 0.05, 1.16 |
No. of reflections | 2964 | 4203 |
No. of parameters | 260 | 388 |
H-atom treatment | All H-atom parameters refined | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.06, −0.50 | 0.87, −0.55 |
Selected geometric parameters (Å, º) for (I) topMg—O1 | 2.056 (4) | Mg—O1 | 2.056 (4) |
Mg—O2 | 2.052 (3) | Mg—O2 | 2.052 (3) |
Mg—N11 | 2.226 (4) | Mg—N11 | 2.226 (4) |
| | | |
O1—Mg—O2 | 85.66 (12) | N11—Mg—O1 | 89.70 (13) |
O1—Mg—N11 | 172.90 (14) | N11—Mg—O2 | 94.13 (13) |
O1—Mg—O1 | 93.28 (15) | N11—Mg—N11 | 88.08 (14) |
O1—Mg—O2 | 92.52 (13) | O1—Mg—O2 | 85.66 (13) |
O1—Mg—N11 | 89.70 (13) | O1—Mg—N11 | 172.90 (14) |
O2—Mg—N11 | 87.78 (12) | O2—Mg—N11 | 87.78 (12) |
O2—Mg—O1 | 92.52 (13) | Mg—N11—C12 | 121.0 (3) |
O2—Mg—O2 | 177.35 (14) | Mg—N11—C16 | 122.8 (2) |
O2—Mg—N11 | 94.13 (13) | | |
Hydrogen-bond geometry (Å, º) for (I) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1B···Ii | 0.76 (5) | 2.88 (4) | 3.601 (3) | 161 (4) |
O2—H2A···Ii | 0.75 (6) | 2.71 (6) | 3.466 (3) | 178 (5) |
Symmetry code: (i) −x+1, y+1, −z+1/2. |
Selected geometric parameters (Å, º) for (II) topSr—I1 | 3.2530 (11) | Sr—N11 | 2.729 (5) |
Sr—I2 | 3.2801 (11) | Sr—N21 | 2.797 (5) |
Sr—O1A | 2.549 (4) | Sr—N11' | 2.764 (5) |
Sr—O1B | 2.592 (4) | | |
| | | |
I1—Sr—I2 | 176.07 (2) | O1A—Sr—O1B | 140.38 (15) |
I1—Sr—O1A | 90.77 (16) | O1A—Sr—N11 | 70.08 (15) |
I1—Sr—O1B | 96.68 (16) | O1A—Sr—N21 | 70.34 (16) |
I1—Sr—N11 | 88.27 (17) | O1A—Sr—N11' | 139.79 (15) |
I1—Sr—N21 | 88.06 (17) | O1B—Sr—N11 | 71.32 (15) |
I1—Sr—N11' | 86.74 (17) | O1B—Sr—N21 | 148.43 (16) |
I2—Sr—O1A | 87.76 (15) | O1B—Sr—N11' | 79.64 (15) |
I2—Sr—O1B | 86.76 (16) | N11—Sr—N21 | 140.18 (16) |
I2—Sr—N11 | 94.66 (17) | N11—Sr—N11' | 149.72 (15) |
I2—Sr—N21 | 88.01 (17) | N21—Sr—N11' | 69.46 (16) |
I2—Sr—N11' | 92.03 (17) | | |
In the course of extended studies undertaken some years ago concerning the synthesis and structural characterization of nitrogen base adducts of simple group 2 salts with simple nitrogen base ligands, a hitherto largely unexplored fundamental field, we investigated derivatives formed between the metal halides and the inherently bridging bidentate ligand 4,4'-bipyridine, in the expectation that unusual polymeric arrays might be obtained (Kepert et al., 1996). In doing so, the metal iodides were dissolved with the ligand in 1:2 millimolar stoichiometry in a few ml of alcoholic solvent (propan-1-ol for the heavier metals, methanol for the lighter) under anaerobic conditions, i.e. specifically excluding moisture. At the time, a crystalline deposit was obtained only of a barium complex, which proved to be an adduct of stoichiometry BaI2:4,4'-bipyridine:propan-1-ol (1:2.5:2), a novel polymer in which seven-coordinate Ba atoms of pentagonal-bipyramidal stereochemistry (environment: BaI2N3O2), comprising the two axial I atoms, three pyridyl N atoms (from different ligands) and two propan-1-ol O atoms, were linked into a one-dimensional double-stranded polymer. After standing for some years, two parallel vials containing magnesium iodide with ligand in methanol, and strontium iodide with ligand in propan-1-ol, deposited significant quantities of colourless well formed crystals, the title complexes, (I) and (II), respectively. The strontium complex, (II), proved to be a counterpart of the previously described barium adduct, while the magnesium complex, (I), is an adduct of the form MgI2-4,4'-bipyridine-water (1:3:4), presumably consequent upon the slow admission of water from the surroundings over an extended period and/or some presence in the initial mixture. In both complexes, coordinated bridging 4,4'-bipyridine moieties are found, so that polymers result. In both compounds, uncoordinated 4,4'-bipyridine moieties are also found, which are prone to stack or interleave interstitially, being (quasi-)planar but not inflexibly so. \sch
In complex (I), one half of the 1:3:4 MgI2-4,4'-bipyridine-water formula unit comprises the asymmetric unit of the structure, the Mg atom being disposed on a crystallographic 2 axis, while the mid-point of the central bond of the coordinated 4,4'-bipyridine ligand lies at a crystallographic centre of symmetry, the two C5N rings necessarily parallel and essentially coplanar, the Mg atom deviant by 0.234 (6) and 0.199 (14) Å. The lattice 4,4'-bipyridine moiety is fully crystallographically independent. The Mg atom environment is six-coordinate and quasi-octahedral in stereochemistry. Symmetry-related 4,4'-bipyridine moieties lie cis in the coordination sphere, bonded through their N atoms and bridging to inversion-related Mg atoms to generate an infinite one-dimensional zigzag polymeric cation along the crystallographic c axis (Fig. 2).
The Mg-coordinated atom distances (Table 1) are unremarkable and are comparable with values recorded for similar bonds in examples of pyridine base and aqua ligand complexes (e.g. Waters & White, 1996), there being no significant difference in the two Mg—OH2 distances indicative of any significant difference in trans effects of the two ligand types.
Although the polymer of (I) is one-dimensional, its profile is extended in the second dimension (b) by its zigzag aspect, with the overall array having a planar core disposed in the bc face of the cell (Fig. 2 b) and the dihedral angle of the C5N ligand plane to that face being 51.0 (1)°. One H atom from each water molecule is involved in a strong hydrogen bond projecting out of the plane to the same nearby iodide ion (Table 2), and these interactions are perhaps responsible for the considerable deviations of the angles about the Mg atom from orthogonality. Whereas the coordinated ligand is essentially planar, the uncoordinated moiety is twisted about its central bond, the dihedral angle between the two C5N planes (χ2 20 and 1) being 33.8 (2)°.
The strontium complex, (II), is isomorphous with its barium counterpart, previously recorded elsewhere (Kepert et al., 1996). One full formula unit, devoid of crystallographic symmetry (but see below), comprises the asymmetric unit of the structure. The coordinated 4,4'-bipyridine complement comprises the two halves of different ligands 1, this ligand bridging to a (b-) unit-translation-related metal atom, and one half of ligand 2, which lies with the midpoint of its central bond disposed at a crystallographic inversion centre. The two rings of the second ligand are necessarily parallel and quasi-coplanar, the metal atom deviating from the C5N plane (χ2 5.6) by 0.34 (1) Å. The two similar component planes (χ2 6.5 and 0.4) of the first ligand lie twisted about the central bond with respect to each other, with an interplanar dihedral angle of 23.0 (4)° and with the associated Sr atoms considerably [0.81 (1) and 1.23 (3) Å] out of plane in each case. [The third uncoordinated ligand is crystallographically fully independent and is also similarly twisted, the interplanar dihedral angle being 33.7 (4)°].
The metal atoms of (II) are seven-coordinate, the coordination environment approximating nicely to pentagonal-bipyramidal stereochemistry, with the I atoms occupying the trans/axial sites. Two of the five equatorial sites (not cis) are occupied by the propan-1-ol ligand O atoms, which thus define the orientation of the other three pyridine N atoms in the I2SrO2N3 coordination sphere. As implied above, two of the N atoms come from the two independent rings of the symmetry-related ligands 1 which extend the resulting polymer in b; the other is from the independent half of ligand 2 which, by inversion, extends the polymer in the second dimension across the cell diagonal. The resulting planar array (Fig. 3a) comprises a double-stranded polymer running parallel to b (Fig. 3 b).
The metal atom environment of (II) may be compared with that of its barium counterpart, in which the Ba—I(1,2)/O(1 A,B)/N(11,21,11') distances are 3.382 (4), 3.403 (4), 2.69 (2), 2.74 (1), 2.85 (2), 2.94 (2) and 2.91 (2) Å, respectively. Thus the mean differences between Ba and Sr bond lengths for I, O and N donors are 0.13, 0.15, 0.14 Å, respectively, suggesting no outstanding differential between bond types.