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Acta Crystallographica Section E: Structure Reports Online logoLink to Acta Crystallographica Section E: Structure Reports Online
. 2011 Jun 25;67(Pt 7):m987. doi: 10.1107/S1600536811023865

Di-μ-chlorido-bis­{[N,N′-dicyclo­hexyl-N′′,N′′-bis­(trimethyl­sil­yl)guanidinato-κ2 N,N′](tetra­hydro­furan-κO)magnesium(II)}

Jie Cheng a,*
PMCID: PMC3152120  PMID: 21836960

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).graphic file with name e-67-0m987-scheme1.jpg

Experimental

Crystal data

  • [Mg2(C19H40N3Si2)2Cl2(C4H8O)2]

  • M r = 997.17

  • Triclinic, Inline graphic

  • 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

e-67-0m987-sup1.cif (28.7KB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811023865/hb5890Isup2.hkl

e-67-0m987-Isup2.hkl (268.5KB, 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) Inline graphic.

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.

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 m3
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 mm1
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 Å3
2 restraints Δρmin = −0.42 e Å3

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

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  3. Jacobson, R. (1998). REQAB Private communication to the Rigaku Corporation, Tokyo, Japan.
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  7. 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

e-67-0m987-sup1.cif (28.7KB, cif)

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811023865/hb5890Isup2.hkl

e-67-0m987-Isup2.hkl (268.5KB, hkl)

Additional supplementary materials: crystallographic information; 3D view; checkCIF report


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