Abstract
The dinuclear title complex, [Mg2(C19H40N3Si2)2Cl2(C4H8O)2], lies on a center of inversion. The Mg2+ ions are bonded to a chelating N,N′-bonded guanidinate anion, a tetrahydrofuran molecule and two bridging chloride anions. The geometry of the resulting five-coordinated Mg2+ ion is a very distorted square-based pyramid with the O atom in the apical position.
Related literature
For the synthesis of analogous metal-ligated complexes, see: Sánchez-Barba et al. (2006 ▶); Doring & Kempe (2009 ▶); Lyubov et al. (2007 ▶). For a review of the crystal structures of guanidinato-ligated metal complexes, see: Bailey & Pace (2001 ▶).
Experimental
Crystal data
[Mg2(C19H40N3Si2)2Cl2(C4H8O)2]
M r = 997.17
Triclinic,
a = 8.7249 (3) Å
b = 11.0016 (5) Å
c = 16.8893 (8) Å
α = 79.487 (6)°
β = 75.211 (6)°
γ = 72.201 (5)°
V = 1482.80 (11) Å3
Z = 1
Mo Kα radiation
μ = 0.25 mm−1
T = 223 K
0.60 × 0.30 × 0.22 mm
Data collection
Rigaku Saturn diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.340, T max = 0.462
12201 measured reflections
5485 independent reflections
4175 reflections with I > 2σ(I)
R int = 0.028
Refinement
R[F 2 > 2σ(F 2)] = 0.050
wR(F 2) = 0.141
S = 1.08
5485 reflections
287 parameters
2 restraints
H-atom parameters constrained
Δρmax = 0.40 e Å−3
Δρmin = −0.42 e Å−3
Data collection: CrystalClear (Rigaku, 2000 ▶); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku, 2000 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.
Supplementary Material
Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811023865/hb5890sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811023865/hb5890Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report
Table 1. Selected bond lengths (Å).
| Mg1—O1 | 2.0334 (19) |
| Mg1—N2 | 2.0734 (18) |
| Mg1—N1 | 2.1247 (17) |
| Mg1—Cl1i | 2.4946 (9) |
| Mg1—Cl1 | 2.4171 (9) |
Symmetry code: (i)
.
Acknowledgments
The author thanks Yong Zhang of Suzhou University for the data collection.
supplementary crystallographic information
Comment
The title compound exists as a centrosymmetric dinuclear molecule in which each Mg2+ is five-coordinated by one bidentate guanidinato anion in h2-fashion, two chlorido anions, and one THF molecule to adopt a distorted pyramidal geometry (Fig. 1). The two {Mg(guanidinato)(THF)}+ moieties are connected by two chlorido anions in m2-mode.
Experimental
The mono(guanidinato) yttrium dichloride complex was synthesized by the reaction of guanidinato lithium with one equivalent of YCl3 in THF according to a literature procedure. Treatment of the mono(guanidinato) yttrium dichloride complex with Mg(C3H5)Cl in 1:2 molar ratio in THF at room temperature, after recrystallization, afforded the title complex as colorless crystals. Colourless prisms were obtained from a saturated hexane solution at 243 K.
Refinement
H-atoms were placed in calculated positions and were included in the refinement in the riding model approximation.
Figures
Fig. 1.
Molecular structure of the title compound with displacement elliposids drawn at the 30% probability level. Atoms with suffix A are generated by the symmetry operation (1–x, 1–y, 1–z).
Crystal data
| [Mg2(C19H40N3Si2)2Cl2(C4H8O)2] | Z = 1 |
| Mr = 997.17 | F(000) = 544 |
| Triclinic, P1 | Dx = 1.117 Mg m−3 |
| Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71075 Å |
| a = 8.7249 (3) Å | Cell parameters from 6219 reflections |
| b = 11.0016 (5) Å | θ = 3.0–27.5° |
| c = 16.8893 (8) Å | µ = 0.25 mm−1 |
| α = 79.487 (6)° | T = 223 K |
| β = 75.211 (6)° | Prism, colourless |
| γ = 72.201 (5)° | 0.60 × 0.30 × 0.22 mm |
| V = 1482.80 (11) Å3 |
Data collection
| Rigaku Saturn diffractometer | 5485 independent reflections |
| Radiation source: fine-focus sealed tube | 4175 reflections with I > 2σ(I) |
| graphite | Rint = 0.028 |
| Detector resolution: 14.63 pixels mm-1 | θmax = 25.5°, θmin = 3.0° |
| ω scans | h = −10→10 |
| Absorption correction: multi-scan (REQAB; Jacobson, 1998) | k = −13→11 |
| Tmin = 0.340, Tmax = 0.462 | l = −20→18 |
| 12201 measured reflections |
Refinement
| 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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.141 | H-atom parameters constrained |
| S = 1.08 | w = 1/[σ2(Fo2) + (0.0855P)2] where P = (Fo2 + 2Fc2)/3 |
| 5485 reflections | (Δ/σ)max = 0.001 |
| 287 parameters | Δρmax = 0.40 e Å−3 |
| 2 restraints | Δρmin = −0.42 e Å−3 |
Special details
| 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)
| x | y | z | Uiso*/Ueq | ||
| Cl1 | 0.57869 (8) | 0.59193 (6) | 0.53865 (3) | 0.0538 (2) | |
| Si1 | 0.19612 (8) | 0.27490 (6) | 0.89356 (3) | 0.04007 (19) | |
| Si2 | 0.57738 (8) | 0.19428 (7) | 0.83044 (4) | 0.0486 (2) | |
| Mg1 | 0.37458 (9) | 0.47603 (7) | 0.60061 (4) | 0.0372 (2) | |
| O1 | 0.1567 (2) | 0.6051 (2) | 0.58704 (11) | 0.0670 (6) | |
| N1 | 0.3601 (2) | 0.47652 (18) | 0.72806 (10) | 0.0400 (4) | |
| N2 | 0.3613 (2) | 0.30543 (17) | 0.67452 (10) | 0.0350 (4) | |
| N3 | 0.3771 (2) | 0.27627 (17) | 0.81889 (9) | 0.0319 (4) | |
| C1 | 0.3639 (2) | 0.3536 (2) | 0.74099 (11) | 0.0308 (4) | |
| C2 | 0.3718 (3) | 0.5451 (2) | 0.79118 (13) | 0.0489 (6) | |
| H2 | 0.3730 | 0.4863 | 0.8431 | 0.059* | |
| C3 | 0.2249 (4) | 0.6613 (3) | 0.80647 (19) | 0.0698 (8) | |
| H3A | 0.1235 | 0.6336 | 0.8224 | 0.084* | |
| H3B | 0.2207 | 0.7198 | 0.7553 | 0.084* | |
| C4 | 0.2330 (5) | 0.7332 (4) | 0.8742 (2) | 0.0911 (12) | |
| H4A | 0.1395 | 0.8102 | 0.8800 | 0.109* | |
| H4B | 0.2250 | 0.6780 | 0.9268 | 0.109* | |
| C5 | 0.3926 (5) | 0.7717 (3) | 0.85416 (16) | 0.0771 (10) | |
| H5A | 0.3921 | 0.8377 | 0.8065 | 0.093* | |
| H5B | 0.4000 | 0.8090 | 0.9011 | 0.093* | |
| C6 | 0.5393 (5) | 0.6602 (4) | 0.8355 (2) | 0.0837 (10) | |
| H6A | 0.5498 | 0.6008 | 0.8859 | 0.100* | |
| H6B | 0.6385 | 0.6907 | 0.8174 | 0.100* | |
| C7 | 0.5280 (4) | 0.5886 (3) | 0.76892 (18) | 0.0670 (8) | |
| H7A | 0.5304 | 0.6449 | 0.7167 | 0.080* | |
| H7B | 0.6238 | 0.5135 | 0.7611 | 0.080* | |
| C8 | 0.3507 (2) | 0.1751 (2) | 0.67767 (12) | 0.0345 (5) | |
| H8 | 0.3583 | 0.1305 | 0.7336 | 0.041* | |
| C9 | 0.4891 (3) | 0.0989 (2) | 0.61505 (13) | 0.0410 (5) | |
| H9A | 0.4838 | 0.1429 | 0.5595 | 0.049* | |
| H9B | 0.5956 | 0.0953 | 0.6258 | 0.049* | |
| C10 | 0.4761 (3) | −0.0373 (2) | 0.61940 (14) | 0.0461 (6) | |
| H10A | 0.5638 | −0.0821 | 0.5769 | 0.055* | |
| H10B | 0.4926 | −0.0838 | 0.6732 | 0.055* | |
| C11 | 0.3108 (3) | −0.0390 (2) | 0.60709 (15) | 0.0490 (6) | |
| H11A | 0.3020 | −0.0058 | 0.5500 | 0.059* | |
| H11B | 0.3031 | −0.1277 | 0.6167 | 0.059* | |
| C12 | 0.1706 (3) | 0.0416 (3) | 0.66506 (18) | 0.0599 (7) | |
| H12A | 0.1683 | −0.0004 | 0.7216 | 0.072* | |
| H12B | 0.0662 | 0.0469 | 0.6512 | 0.072* | |
| C13 | 0.1866 (3) | 0.1767 (3) | 0.66063 (18) | 0.0534 (6) | |
| H13A | 0.0963 | 0.2239 | 0.7011 | 0.064* | |
| H13B | 0.1770 | 0.2220 | 0.6057 | 0.064* | |
| C14 | 0.0156 (3) | 0.3832 (3) | 0.85500 (17) | 0.0582 (7) | |
| H14A | 0.0309 | 0.4687 | 0.8390 | 0.087* | |
| H14B | −0.0829 | 0.3867 | 0.8981 | 0.087* | |
| H14C | 0.0040 | 0.3510 | 0.8077 | 0.087* | |
| C15 | 0.1996 (4) | 0.3282 (4) | 0.99136 (16) | 0.0809 (10) | |
| H15A | 0.2800 | 0.2636 | 1.0181 | 0.121* | |
| H15B | 0.0915 | 0.3401 | 1.0276 | 0.121* | |
| H15C | 0.2293 | 0.4088 | 0.9794 | 0.121* | |
| C16 | 0.1665 (4) | 0.1109 (3) | 0.9186 (2) | 0.0867 (11) | |
| H16A | 0.1686 | 0.0788 | 0.8684 | 0.130* | |
| H16B | 0.0612 | 0.1141 | 0.9563 | 0.130* | |
| H16C | 0.2543 | 0.0543 | 0.9442 | 0.130* | |
| C17 | 0.7269 (3) | 0.2293 (3) | 0.73586 (18) | 0.0684 (8) | |
| H17A | 0.7127 | 0.1940 | 0.6905 | 0.103* | |
| H17B | 0.8381 | 0.1907 | 0.7446 | 0.103* | |
| H17C | 0.7085 | 0.3215 | 0.7229 | 0.103* | |
| C18 | 0.6256 (4) | 0.2438 (5) | 0.9186 (2) | 0.1038 (14) | |
| H18A | 0.6050 | 0.3364 | 0.9120 | 0.156* | |
| H18B | 0.7405 | 0.2035 | 0.9203 | 0.156* | |
| H18C | 0.5564 | 0.2172 | 0.9696 | 0.156* | |
| C19 | 0.6096 (5) | 0.0173 (4) | 0.8484 (4) | 0.129 (2) | |
| H19A | 0.5437 | −0.0052 | 0.9016 | 0.193* | |
| H19B | 0.7251 | −0.0249 | 0.8477 | 0.193* | |
| H19C | 0.5770 | −0.0103 | 0.8054 | 0.193* | |
| C20 | 0.0019 (4) | 0.6055 (4) | 0.6432 (2) | 0.0992 (13) | |
| H20A | 0.0158 | 0.5861 | 0.7004 | 0.119* | |
| H20B | −0.0449 | 0.5418 | 0.6317 | 0.119* | |
| C21 | −0.1037 (6) | 0.7348 (6) | 0.6292 (4) | 0.172 (3) | |
| H21A | −0.2109 | 0.7309 | 0.6234 | 0.206* | |
| H21B | −0.1217 | 0.7818 | 0.6763 | 0.206* | |
| C22 | −0.0259 (5) | 0.8007 (4) | 0.5551 (3) | 0.1056 (13) | |
| H22A | −0.0022 | 0.8755 | 0.5680 | 0.127* | |
| H22B | −0.0981 | 0.8299 | 0.5155 | 0.127* | |
| C23 | 0.1279 (4) | 0.7076 (4) | 0.5207 (2) | 0.0896 (11) | |
| H23A | 0.1160 | 0.6748 | 0.4731 | 0.108* | |
| H23B | 0.2192 | 0.7475 | 0.5035 | 0.108* |
Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Cl1 | 0.0806 (4) | 0.0615 (4) | 0.0290 (3) | −0.0396 (4) | −0.0038 (3) | −0.0054 (2) |
| Si1 | 0.0467 (4) | 0.0415 (4) | 0.0285 (3) | −0.0158 (3) | 0.0035 (2) | −0.0051 (2) |
| Si2 | 0.0422 (4) | 0.0536 (5) | 0.0536 (4) | −0.0178 (3) | −0.0203 (3) | 0.0075 (3) |
| Mg1 | 0.0451 (4) | 0.0361 (4) | 0.0264 (3) | −0.0095 (3) | −0.0043 (3) | −0.0013 (3) |
| O1 | 0.0567 (11) | 0.0719 (14) | 0.0464 (10) | 0.0067 (10) | −0.0073 (8) | 0.0108 (9) |
| N1 | 0.0589 (11) | 0.0359 (11) | 0.0257 (8) | −0.0166 (9) | −0.0045 (8) | −0.0043 (7) |
| N2 | 0.0435 (9) | 0.0367 (11) | 0.0259 (8) | −0.0128 (8) | −0.0048 (7) | −0.0068 (7) |
| N3 | 0.0367 (9) | 0.0354 (10) | 0.0248 (8) | −0.0143 (8) | −0.0046 (7) | −0.0015 (7) |
| C1 | 0.0288 (9) | 0.0373 (13) | 0.0249 (9) | −0.0097 (9) | −0.0020 (7) | −0.0041 (8) |
| C2 | 0.0848 (17) | 0.0400 (14) | 0.0270 (10) | −0.0288 (13) | −0.0077 (11) | −0.0023 (9) |
| C3 | 0.0805 (19) | 0.060 (2) | 0.0731 (18) | −0.0304 (16) | 0.0093 (15) | −0.0344 (15) |
| C4 | 0.138 (3) | 0.071 (2) | 0.0680 (19) | −0.051 (2) | 0.019 (2) | −0.0372 (17) |
| C5 | 0.149 (3) | 0.059 (2) | 0.0388 (13) | −0.057 (2) | −0.0124 (17) | −0.0067 (13) |
| C6 | 0.122 (3) | 0.088 (3) | 0.0692 (19) | −0.054 (2) | −0.0325 (19) | −0.0161 (18) |
| C7 | 0.0733 (18) | 0.076 (2) | 0.0661 (17) | −0.0309 (16) | −0.0113 (14) | −0.0298 (15) |
| C8 | 0.0399 (11) | 0.0360 (13) | 0.0280 (10) | −0.0122 (10) | −0.0033 (8) | −0.0067 (8) |
| C9 | 0.0394 (11) | 0.0417 (14) | 0.0380 (11) | −0.0068 (10) | −0.0025 (9) | −0.0104 (10) |
| C10 | 0.0527 (13) | 0.0371 (14) | 0.0386 (12) | −0.0003 (11) | −0.0034 (10) | −0.0091 (10) |
| C11 | 0.0583 (14) | 0.0389 (14) | 0.0511 (13) | −0.0129 (12) | −0.0058 (11) | −0.0177 (11) |
| C12 | 0.0471 (13) | 0.0624 (19) | 0.0775 (18) | −0.0236 (13) | 0.0025 (13) | −0.0336 (14) |
| C13 | 0.0388 (12) | 0.0507 (16) | 0.0746 (17) | −0.0090 (11) | −0.0037 (12) | −0.0340 (13) |
| C14 | 0.0399 (12) | 0.071 (2) | 0.0605 (15) | −0.0193 (13) | 0.0009 (11) | −0.0078 (13) |
| C15 | 0.0731 (19) | 0.133 (3) | 0.0381 (14) | −0.033 (2) | 0.0053 (13) | −0.0294 (17) |
| C16 | 0.095 (2) | 0.054 (2) | 0.086 (2) | −0.0323 (17) | 0.0359 (19) | −0.0026 (16) |
| C17 | 0.0346 (12) | 0.091 (2) | 0.0725 (18) | −0.0094 (14) | −0.0023 (12) | −0.0195 (16) |
| C18 | 0.0684 (19) | 0.196 (5) | 0.0614 (19) | −0.042 (2) | −0.0300 (16) | −0.017 (2) |
| C19 | 0.080 (2) | 0.058 (2) | 0.253 (6) | −0.0194 (19) | −0.087 (3) | 0.045 (3) |
| C20 | 0.0543 (18) | 0.118 (3) | 0.092 (2) | −0.0068 (19) | −0.0064 (17) | 0.028 (2) |
| C21 | 0.092 (3) | 0.161 (5) | 0.151 (5) | 0.055 (3) | 0.015 (3) | 0.044 (4) |
| C22 | 0.095 (3) | 0.083 (3) | 0.117 (3) | 0.011 (2) | −0.042 (2) | 0.010 (2) |
| C23 | 0.090 (2) | 0.087 (3) | 0.067 (2) | −0.001 (2) | −0.0260 (17) | 0.0263 (18) |
Geometric parameters (Å, °)
| Si1—N3 | 1.7532 (16) | C9—H9A | 0.9800 |
| Si1—C14 | 1.849 (3) | C9—H9B | 0.9800 |
| Si1—C16 | 1.857 (3) | C10—C11 | 1.515 (3) |
| Si1—C15 | 1.861 (3) | C10—H10A | 0.9800 |
| Si2—N3 | 1.7472 (18) | C10—H10B | 0.9800 |
| Si2—C17 | 1.850 (3) | C11—C12 | 1.511 (3) |
| Si2—C18 | 1.857 (3) | C11—H11A | 0.9800 |
| Si2—C19 | 1.858 (4) | C11—H11B | 0.9800 |
| Mg1—O1 | 2.0334 (19) | C12—C13 | 1.523 (4) |
| Mg1—N2 | 2.0734 (18) | C12—H12A | 0.9800 |
| Mg1—N1 | 2.1247 (17) | C12—H12B | 0.9800 |
| Mg1—Cl1i | 2.4946 (9) | C13—H13A | 0.9800 |
| Mg1—Cl1 | 2.4171 (9) | C13—H13B | 0.9800 |
| Mg1—Mg1i | 3.5878 (13) | C14—H14A | 0.9700 |
| O1—C20 | 1.439 (4) | C14—H14B | 0.9700 |
| O1—C23 | 1.449 (3) | C14—H14C | 0.9700 |
| N1—C1 | 1.321 (3) | C15—H15A | 0.9700 |
| N1—C2 | 1.453 (3) | C15—H15B | 0.9700 |
| N2—C1 | 1.334 (3) | C15—H15C | 0.9700 |
| N2—C8 | 1.455 (3) | C16—H16A | 0.9700 |
| N3—C1 | 1.441 (2) | C16—H16B | 0.9700 |
| C2—C3 | 1.515 (4) | C16—H16C | 0.9700 |
| C2—C7 | 1.516 (4) | C17—H17A | 0.9700 |
| C2—H2 | 0.9900 | C17—H17B | 0.9700 |
| C3—C4 | 1.531 (4) | C17—H17C | 0.9700 |
| C3—H3A | 0.9800 | C18—H18A | 0.9700 |
| C3—H3B | 0.9800 | C18—H18B | 0.9700 |
| C4—C5 | 1.517 (5) | C18—H18C | 0.9700 |
| C4—H4A | 0.9800 | C19—H19A | 0.9700 |
| C4—H4B | 0.9800 | C19—H19B | 0.9700 |
| C5—C6 | 1.489 (5) | C19—H19C | 0.9700 |
| C5—H5A | 0.9800 | C20—C21 | 1.455 (6) |
| C5—H5B | 0.9800 | C20—H20A | 0.9800 |
| C6—C7 | 1.524 (4) | C20—H20B | 0.9800 |
| C6—H6A | 0.9800 | C21—C22 | 1.445 (6) |
| C6—H6B | 0.9800 | C21—H21A | 0.9800 |
| C7—H7A | 0.9800 | C21—H21B | 0.9800 |
| C7—H7B | 0.9800 | C22—C23 | 1.471 (5) |
| C8—C13 | 1.525 (3) | C22—H22A | 0.9800 |
| C8—C9 | 1.527 (3) | C22—H22B | 0.9800 |
| C8—H8 | 0.9900 | C23—H23A | 0.9800 |
| C9—C10 | 1.525 (3) | C23—H23B | 0.9800 |
| Mg1—Cl1—Mg1i | 93.84 (3) | C13—C8—H8 | 108.6 |
| N3—Si1—C14 | 110.04 (10) | C9—C8—H8 | 108.6 |
| N3—Si1—C16 | 111.06 (12) | C10—C9—C8 | 111.38 (17) |
| C14—Si1—C16 | 108.07 (16) | C10—C9—H9A | 109.4 |
| N3—Si1—C15 | 111.90 (11) | C8—C9—H9A | 109.4 |
| C14—Si1—C15 | 108.22 (15) | C10—C9—H9B | 109.4 |
| C16—Si1—C15 | 107.41 (18) | C8—C9—H9B | 109.4 |
| N3—Si2—C17 | 109.83 (11) | H9A—C9—H9B | 108.0 |
| N3—Si2—C18 | 111.12 (14) | C11—C10—C9 | 112.2 (2) |
| C17—Si2—C18 | 108.39 (16) | C11—C10—H10A | 109.2 |
| N3—Si2—C19 | 112.06 (12) | C9—C10—H10A | 109.2 |
| C17—Si2—C19 | 107.5 (2) | C11—C10—H10B | 109.2 |
| C18—Si2—C19 | 107.8 (2) | C9—C10—H10B | 109.2 |
| O1—Mg1—N2 | 116.59 (8) | H10A—C10—H10B | 107.9 |
| O1—Mg1—N1 | 100.44 (8) | C12—C11—C10 | 111.19 (19) |
| N2—Mg1—N1 | 64.10 (7) | C12—C11—H11A | 109.4 |
| O1—Mg1—Cl1 | 104.41 (7) | C10—C11—H11A | 109.4 |
| N2—Mg1—Cl1 | 138.03 (6) | C12—C11—H11B | 109.4 |
| N1—Mg1—Cl1 | 101.29 (6) | C10—C11—H11B | 109.4 |
| O1—Mg1—Cl1i | 91.66 (6) | H11A—C11—H11B | 108.0 |
| N2—Mg1—Cl1i | 100.61 (5) | C11—C12—C13 | 112.2 (2) |
| N1—Mg1—Cl1i | 163.61 (6) | C11—C12—H12A | 109.2 |
| Cl1—Mg1—Cl1i | 86.16 (3) | C13—C12—H12A | 109.2 |
| O1—Mg1—C1 | 113.31 (7) | C11—C12—H12B | 109.2 |
| N2—Mg1—C1 | 32.25 (7) | C13—C12—H12B | 109.2 |
| N1—Mg1—C1 | 31.92 (7) | H12A—C12—H12B | 107.9 |
| Cl1—Mg1—C1 | 122.25 (5) | C12—C13—C8 | 111.8 (2) |
| Cl1i—Mg1—C1 | 132.33 (6) | C12—C13—H13A | 109.3 |
| O1—Mg1—Mg1i | 100.82 (6) | C8—C13—H13A | 109.3 |
| N2—Mg1—Mg1i | 128.97 (6) | C12—C13—H13B | 109.3 |
| N1—Mg1—Mg1i | 143.03 (6) | C8—C13—H13B | 109.3 |
| Cl1—Mg1—Mg1i | 43.93 (2) | H13A—C13—H13B | 107.9 |
| Cl1i—Mg1—Mg1i | 42.236 (19) | Si1—C14—H14A | 109.5 |
| C1—Mg1—Mg1i | 145.86 (6) | Si1—C14—H14B | 109.5 |
| C20—O1—C23 | 108.6 (2) | H14A—C14—H14B | 109.5 |
| C20—O1—Mg1 | 123.90 (18) | Si1—C14—H14C | 109.5 |
| C23—O1—Mg1 | 127.48 (18) | H14A—C14—H14C | 109.5 |
| C1—N1—C2 | 122.68 (17) | H14B—C14—H14C | 109.5 |
| C1—N1—Mg1 | 89.82 (12) | Si1—C15—H15A | 109.5 |
| C2—N1—Mg1 | 146.53 (14) | Si1—C15—H15B | 109.5 |
| C1—N2—C8 | 122.48 (17) | H15A—C15—H15B | 109.5 |
| C1—N2—Mg1 | 91.70 (13) | Si1—C15—H15C | 109.5 |
| C8—N2—Mg1 | 145.82 (13) | H15A—C15—H15C | 109.5 |
| C1—N3—Si2 | 115.52 (12) | H15B—C15—H15C | 109.5 |
| C1—N3—Si1 | 118.56 (13) | Si1—C16—H16A | 109.5 |
| Si2—N3—Si1 | 125.91 (10) | Si1—C16—H16B | 109.5 |
| N1—C1—N2 | 114.12 (17) | H16A—C16—H16B | 109.5 |
| N1—C1—N3 | 123.27 (17) | Si1—C16—H16C | 109.5 |
| N2—C1—N3 | 122.56 (18) | H16A—C16—H16C | 109.5 |
| N1—C1—Mg1 | 58.25 (10) | H16B—C16—H16C | 109.5 |
| N2—C1—Mg1 | 56.05 (10) | Si2—C17—H17A | 109.5 |
| N3—C1—Mg1 | 173.59 (14) | Si2—C17—H17B | 109.5 |
| N1—C2—C3 | 111.2 (2) | H17A—C17—H17B | 109.5 |
| N1—C2—C7 | 112.17 (19) | Si2—C17—H17C | 109.5 |
| C3—C2—C7 | 108.8 (2) | H17A—C17—H17C | 109.5 |
| N1—C2—H2 | 108.2 | H17B—C17—H17C | 109.5 |
| C3—C2—H2 | 108.2 | Si2—C18—H18A | 109.5 |
| C7—C2—H2 | 108.2 | Si2—C18—H18B | 109.5 |
| C2—C3—C4 | 112.0 (3) | H18A—C18—H18B | 109.5 |
| C2—C3—H3A | 109.2 | Si2—C18—H18C | 109.5 |
| C4—C3—H3A | 109.2 | H18A—C18—H18C | 109.5 |
| C2—C3—H3B | 109.2 | H18B—C18—H18C | 109.5 |
| C4—C3—H3B | 109.2 | Si2—C19—H19A | 109.5 |
| H3A—C3—H3B | 107.9 | Si2—C19—H19B | 109.5 |
| C5—C4—C3 | 111.0 (2) | H19A—C19—H19B | 109.5 |
| C5—C4—H4A | 109.4 | Si2—C19—H19C | 109.5 |
| C3—C4—H4A | 109.4 | H19A—C19—H19C | 109.5 |
| C5—C4—H4B | 109.4 | H19B—C19—H19C | 109.5 |
| C3—C4—H4B | 109.4 | O1—C20—C21 | 105.0 (3) |
| H4A—C4—H4B | 108.0 | O1—C20—H20A | 110.7 |
| C6—C5—C4 | 111.9 (3) | C21—C20—H20A | 110.7 |
| C6—C5—H5A | 109.2 | O1—C20—H20B | 110.7 |
| C4—C5—H5A | 109.2 | C21—C20—H20B | 110.7 |
| C6—C5—H5B | 109.2 | H20A—C20—H20B | 108.8 |
| C4—C5—H5B | 109.2 | C22—C21—C20 | 109.2 (3) |
| H5A—C5—H5B | 107.9 | C22—C21—H21A | 109.8 |
| C5—C6—C7 | 112.3 (3) | C20—C21—H21A | 109.8 |
| C5—C6—H6A | 109.1 | C22—C21—H21B | 109.8 |
| C7—C6—H6A | 109.1 | C20—C21—H21B | 109.8 |
| C5—C6—H6B | 109.1 | H21A—C21—H21B | 108.3 |
| C7—C6—H6B | 109.1 | C21—C22—C23 | 106.6 (3) |
| H6A—C6—H6B | 107.9 | C21—C22—H22A | 110.4 |
| C2—C7—C6 | 111.8 (2) | C23—C22—H22A | 110.4 |
| C2—C7—H7A | 109.3 | C21—C22—H22B | 110.4 |
| C6—C7—H7A | 109.3 | C23—C22—H22B | 110.4 |
| C2—C7—H7B | 109.3 | H22A—C22—H22B | 108.6 |
| C6—C7—H7B | 109.3 | O1—C23—C22 | 105.1 (3) |
| H7A—C7—H7B | 107.9 | O1—C23—H23A | 110.7 |
| N2—C8—C13 | 110.59 (19) | C22—C23—H23A | 110.7 |
| N2—C8—C9 | 112.16 (16) | O1—C23—H23B | 110.7 |
| C13—C8—C9 | 108.22 (17) | C22—C23—H23B | 110.7 |
| N2—C8—H8 | 108.6 | H23A—C23—H23B | 108.8 |
| Mg1i—Cl1—Mg1—O1 | −90.73 (7) | Mg1—N2—C1—N1 | 4.89 (18) |
| Mg1i—Cl1—Mg1—N2 | 101.63 (9) | C8—N2—C1—N3 | 7.9 (3) |
| Mg1i—Cl1—Mg1—N1 | 165.26 (7) | Mg1—N2—C1—N3 | −172.51 (15) |
| Mg1i—Cl1—Mg1—Cl1i | 0.0 | C8—N2—C1—Mg1 | −179.6 (2) |
| Mg1i—Cl1—Mg1—C1 | 139.09 (7) | Si2—N3—C1—N1 | −91.9 (2) |
| N2—Mg1—O1—C20 | 20.7 (3) | Si1—N3—C1—N1 | 86.6 (2) |
| N1—Mg1—O1—C20 | −45.5 (3) | Si2—N3—C1—N2 | 85.2 (2) |
| Cl1—Mg1—O1—C20 | −150.1 (3) | Si1—N3—C1—N2 | −96.2 (2) |
| Cl1i—Mg1—O1—C20 | 123.4 (3) | Si2—N3—C1—Mg1 | 9.8 (13) |
| C1—Mg1—O1—C20 | −14.8 (3) | Si1—N3—C1—Mg1 | −171.7 (12) |
| Mg1i—Mg1—O1—C20 | 165.0 (3) | O1—Mg1—C1—N1 | −71.43 (15) |
| N2—Mg1—O1—C23 | −157.5 (3) | N2—Mg1—C1—N1 | −174.75 (19) |
| N1—Mg1—O1—C23 | 136.3 (3) | Cl1—Mg1—C1—N1 | 54.89 (14) |
| Cl1—Mg1—O1—C23 | 31.7 (3) | Cl1i—Mg1—C1—N1 | 172.78 (11) |
| Cl1i—Mg1—O1—C23 | −54.8 (3) | Mg1i—Mg1—C1—N1 | 108.96 (15) |
| C1—Mg1—O1—C23 | 167.0 (3) | O1—Mg1—C1—N2 | 103.33 (14) |
| Mg1i—Mg1—O1—C23 | −13.3 (3) | N1—Mg1—C1—N2 | 174.75 (19) |
| O1—Mg1—N1—C1 | 117.72 (13) | Cl1—Mg1—C1—N2 | −130.35 (11) |
| N2—Mg1—N1—C1 | 3.11 (11) | Cl1i—Mg1—C1—N2 | −12.46 (14) |
| Cl1—Mg1—N1—C1 | −135.13 (12) | Mg1i—Mg1—C1—N2 | −76.29 (15) |
| Cl1i—Mg1—N1—C1 | −19.2 (3) | O1—Mg1—C1—N3 | −177.1 (12) |
| Mg1i—Mg1—N1—C1 | −118.06 (13) | N2—Mg1—C1—N3 | 79.5 (13) |
| O1—Mg1—N1—C2 | −75.3 (3) | N1—Mg1—C1—N3 | −105.7 (13) |
| N2—Mg1—N1—C2 | 170.1 (3) | Cl1—Mg1—C1—N3 | −50.8 (13) |
| Cl1—Mg1—N1—C2 | 31.8 (3) | Cl1i—Mg1—C1—N3 | 67.1 (13) |
| Cl1i—Mg1—N1—C2 | 147.7 (3) | Mg1i—Mg1—C1—N3 | 3.3 (13) |
| C1—Mg1—N1—C2 | 167.0 (4) | C1—N1—C2—C3 | −123.4 (2) |
| Mg1i—Mg1—N1—C2 | 48.9 (3) | Mg1—N1—C2—C3 | 72.2 (3) |
| O1—Mg1—N2—C1 | −92.06 (13) | C1—N1—C2—C7 | 114.6 (2) |
| N1—Mg1—N2—C1 | −3.08 (11) | Mg1—N1—C2—C7 | −49.9 (4) |
| Cl1—Mg1—N2—C1 | 74.54 (14) | N1—C2—C3—C4 | 178.7 (2) |
| Cl1i—Mg1—N2—C1 | 170.66 (11) | C7—C2—C3—C4 | −57.3 (3) |
| Mg1i—Mg1—N2—C1 | 135.47 (11) | C2—C3—C4—C5 | 55.8 (4) |
| O1—Mg1—N2—C8 | 87.3 (3) | C3—C4—C5—C6 | −52.8 (4) |
| N1—Mg1—N2—C8 | 176.3 (3) | C4—C5—C6—C7 | 53.0 (4) |
| Cl1—Mg1—N2—C8 | −106.1 (2) | N1—C2—C7—C6 | −179.9 (3) |
| Cl1i—Mg1—N2—C8 | −10.0 (3) | C3—C2—C7—C6 | 56.7 (3) |
| C1—Mg1—N2—C8 | 179.4 (3) | C5—C6—C7—C2 | −55.7 (4) |
| Mg1i—Mg1—N2—C8 | −45.1 (3) | C1—N2—C8—C13 | 113.1 (2) |
| C17—Si2—N3—C1 | −0.02 (19) | Mg1—N2—C8—C13 | −66.2 (3) |
| C18—Si2—N3—C1 | 119.9 (2) | C1—N2—C8—C9 | −126.0 (2) |
| C19—Si2—N3—C1 | −119.5 (2) | Mg1—N2—C8—C9 | 54.7 (3) |
| C17—Si2—N3—Si1 | −178.41 (14) | N2—C8—C9—C10 | 179.88 (18) |
| C18—Si2—N3—Si1 | −58.5 (2) | C13—C8—C9—C10 | −57.9 (2) |
| C19—Si2—N3—Si1 | 62.1 (2) | C8—C9—C10—C11 | 56.5 (2) |
| C14—Si1—N3—C1 | −1.54 (18) | C9—C10—C11—C12 | −52.5 (3) |
| C16—Si1—N3—C1 | 118.1 (2) | C10—C11—C12—C13 | 52.2 (3) |
| C15—Si1—N3—C1 | −121.89 (19) | C11—C12—C13—C8 | −56.2 (3) |
| C14—Si1—N3—Si2 | 176.82 (13) | N2—C8—C13—C12 | −178.95 (19) |
| C16—Si1—N3—Si2 | −63.56 (19) | C9—C8—C13—C12 | 57.8 (3) |
| C15—Si1—N3—Si2 | 56.46 (19) | C23—O1—C20—C21 | −22.1 (5) |
| C2—N1—C1—N2 | −176.27 (19) | Mg1—O1—C20—C21 | 159.4 (4) |
| Mg1—N1—C1—N2 | −4.77 (17) | O1—C20—C21—C22 | 11.9 (7) |
| C2—N1—C1—N3 | 1.1 (3) | C20—C21—C22—C23 | 2.5 (7) |
| Mg1—N1—C1—N3 | 172.61 (16) | C20—O1—C23—C22 | 23.7 (4) |
| C2—N1—C1—Mg1 | −171.5 (2) | Mg1—O1—C23—C22 | −157.8 (3) |
| C8—N2—C1—N1 | −174.70 (18) | C21—C22—C23—O1 | −15.7 (6) |
Symmetry codes: (i) −x+1, −y+1, −z+1.
Footnotes
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB5890).
References
- Bailey, P. J. & Pace, S. (2001). Coord. Chem. Rev. 214, 91–141.
- Doring, C. & Kempe, R. (2009). Eur. J. Inorg. Chem. pp. 412–418.
- Jacobson, R. (1998). REQAB Private communication to the Rigaku Corporation, Tokyo, Japan.
- Lyubov, D. M., Fukin, G. K. & Trifonov, A. A. (2007). Inorg Chem. 46, 11450–11456. [DOI] [PubMed]
- Rigaku (2000). CrystalClear and CrystalStructure Rigaku Corporation, Tokyo, Japan.
- Sánchez-Barba, L. F., Hughes, D. L., Humphrey, S. M. & Bochmann, M. (2006). Organometallics, 25, 1012–1020.
- Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [DOI] [PubMed]
Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536811023865/hb5890sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811023865/hb5890Isup2.hkl
Additional supplementary materials: crystallographic information; 3D view; checkCIF report

