Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807052440/ng2346sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807052440/ng2346Isup2.hkl |
CCDC reference: 672727
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.064
- wR factor = 0.161
- Data-to-parameter ratio = 16.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT413_ALERT_2_B Short Inter XH3 .. XHn H8C .. H8C .. 2.05 Ang.
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) 500 Ang. PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 500 Deg. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.38 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for N4 - C24 .. 5.67 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn1 - Si2 .. 7.94 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn1 - N2 .. 5.67 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn2 - Si3 .. 6.85 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn2 - Si4 .. 6.43 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn2 - N6 .. 5.82 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Si1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2 PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C7 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C8 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C19 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C32 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C43 PLAT412_ALERT_2_C Short Intra XH3 .. XHn H20C .. H21B .. 1.81 Ang. PLAT412_ALERT_2_C Short Intra XH3 .. XHn H31C .. H34B .. 1.85 Ang. PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 38.03 Deg. N3 -SI2 -ZN1 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.42 Deg. N5 -SI3 -ZN2 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 37.46 Deg. N7 -SI4 -ZN2 1.555 1.555 1.555
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn1 (2) 1.60 PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn2 (2) 1.60
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 23 ALERT level C = Check and explain 4 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 15 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check
The title compound displays square-planar coordination. Related compounds show linear and tetrahedral coordinations, see: Schumann et al. (2000); Engelhardt et al. (1991). For the applications of zinc amides, see: Amstrong et al. (2002) and for their sythesis by MOVCD, see: Maile et al. (2005).
A solution of LinBu in hexane (2.8 M, 1.9 ml, 5.37 mmol) was added into a solution of [NH(SiMe2NMe2)(2,6-Me2C6H3)] (1.22 g, 5.37 mmol) in Et2O (25 ml) at 273 K. The mixture was stirred at room temperature for 2 h and then ZnCl2 (0.61 g, 2.70 mmol) was added at 273 K. The resulting solution was stirred at room temperature overnight. The filtered solution was concentrated to give the title compound as colorless crystals. Yield: 0.72 g (53%).
The methyl H atoms were then constrained to an ideal geometry, with C—H distances of 0.96 Å and Uiso(H) = 1.2Ueq(C), but each group was allowed to rotate freely about its C–C bond. The other H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms, with C—H distances in the range 0.93Å and Uiso(H) = 1.2Ueq(C).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
Fig. 1. The molecular structure, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted. |
[Zn(C12H21N2Si)2] | Z = 4 |
Mr = 508.17 | F(000) = 1088 |
Triclinic, P1 | Dx = 1.234 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 9.600 (5) Å | Cell parameters from 2236 reflections |
b = 10.447 (5) Å | θ = 2.3–24.1° |
c = 27.338 (5) Å | µ = 1.00 mm−1 |
α = 88.654 (5)° | T = 293 K |
β = 86.151 (5)° | Block, yellow |
γ = 89.858 (5)° | 0.25 × 0.20 × 0.20 mm |
V = 2735 (2) Å3 |
Bruker SMART area-detector diffractometer | 9429 independent reflections |
Radiation source: fine-focus sealed tube | 5229 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→6 |
Tmin = 0.788, Tmax = 0.825 | k = −12→12 |
11316 measured reflections | l = −32→31 |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.161 | H-atom parameters constrained |
S = 0.90 | w = 1/[σ2(Fo2) + (0.0712P)2] where P = (Fo2 + 2Fc2)/3 |
9429 reflections | (Δ/σ)max = 0.001 |
559 parameters | Δρmax = 0.83 e Å−3 |
0 restraints | Δρmin = −0.61 e Å−3 |
[Zn(C12H21N2Si)2] | γ = 89.858 (5)° |
Mr = 508.17 | V = 2735 (2) Å3 |
Triclinic, P1 | Z = 4 |
a = 9.600 (5) Å | Mo Kα radiation |
b = 10.447 (5) Å | µ = 1.00 mm−1 |
c = 27.338 (5) Å | T = 293 K |
α = 88.654 (5)° | 0.25 × 0.20 × 0.20 mm |
β = 86.151 (5)° |
Bruker SMART area-detector diffractometer | 9429 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 5229 reflections with I > 2σ(I) |
Tmin = 0.788, Tmax = 0.825 | Rint = 0.039 |
11316 measured reflections |
R[F2 > 2σ(F2)] = 0.064 | 0 restraints |
wR(F2) = 0.161 | H-atom parameters constrained |
S = 0.90 | Δρmax = 0.83 e Å−3 |
9429 reflections | Δρmin = −0.61 e Å−3 |
559 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
C1 | 1.0352 (5) | 0.6368 (5) | 0.3752 (2) | 0.0338 (13) | |
C2 | 1.1110 (6) | 0.6002 (5) | 0.3311 (2) | 0.0420 (15) | |
C3 | 1.2407 (7) | 0.5422 (6) | 0.3349 (3) | 0.064 (2) | |
H3A | 1.2900 | 0.5162 | 0.3064 | 0.077* | |
C4 | 1.2982 (7) | 0.5218 (6) | 0.3782 (3) | 0.067 (2) | |
H4A | 1.3845 | 0.4816 | 0.3791 | 0.080* | |
C5 | 1.2288 (7) | 0.5608 (6) | 0.4207 (3) | 0.0572 (18) | |
H5A | 1.2694 | 0.5489 | 0.4504 | 0.069* | |
C6 | 1.0982 (6) | 0.6178 (5) | 0.4196 (2) | 0.0418 (15) | |
C7 | 1.0520 (7) | 0.6223 (6) | 0.2833 (2) | 0.071 (2) | |
H7A | 1.1165 | 0.5925 | 0.2577 | 0.106* | |
H7B | 1.0355 | 0.7122 | 0.2784 | 0.106* | |
H7C | 0.9655 | 0.5766 | 0.2827 | 0.106* | |
C8 | 1.0288 (7) | 0.6650 (6) | 0.4672 (2) | 0.0624 (19) | |
H8A | 0.9398 | 0.7021 | 0.4611 | 0.094* | |
H8B | 1.0868 | 0.7285 | 0.4804 | 0.094* | |
H8C | 1.0158 | 0.5945 | 0.4902 | 0.094* | |
C9 | 0.7235 (7) | 0.4972 (6) | 0.3337 (3) | 0.094 (3) | |
H9A | 0.6774 | 0.4248 | 0.3497 | 0.141* | |
H9B | 0.8136 | 0.4717 | 0.3199 | 0.141* | |
H9C | 0.6685 | 0.5294 | 0.3080 | 0.141* | |
C10 | 0.6932 (8) | 0.5531 (8) | 0.4405 (3) | 0.111 (3) | |
H10A | 0.6541 | 0.4697 | 0.4367 | 0.166* | |
H10B | 0.6250 | 0.6068 | 0.4572 | 0.166* | |
H10C | 0.7739 | 0.5458 | 0.4593 | 0.166* | |
C11 | 0.5859 (7) | 0.7736 (6) | 0.3195 (3) | 0.075 (2) | |
H11A | 0.4975 | 0.7307 | 0.3197 | 0.113* | |
H11B | 0.6499 | 0.7366 | 0.2953 | 0.113* | |
H11C | 0.5736 | 0.8629 | 0.3117 | 0.113* | |
C12 | 0.5408 (7) | 0.8041 (6) | 0.4062 (3) | 0.079 (3) | |
H12A | 0.4549 | 0.7577 | 0.4051 | 0.119* | |
H12B | 0.5235 | 0.8939 | 0.4013 | 0.119* | |
H12C | 0.5783 | 0.7898 | 0.4375 | 0.119* | |
C13 | 0.7081 (5) | 1.1005 (5) | 0.3849 (2) | 0.0330 (13) | |
C14 | 0.6785 (6) | 1.1050 (6) | 0.4358 (2) | 0.0508 (17) | |
C15 | 0.5536 (8) | 1.1586 (6) | 0.4535 (3) | 0.067 (2) | |
H15A | 0.5339 | 1.1608 | 0.4873 | 0.080* | |
C16 | 0.4586 (7) | 1.2082 (7) | 0.4235 (3) | 0.072 (2) | |
H16A | 0.3765 | 1.2453 | 0.4365 | 0.087* | |
C17 | 0.4865 (6) | 1.2022 (5) | 0.3738 (3) | 0.0545 (18) | |
H17A | 0.4210 | 1.2330 | 0.3529 | 0.065* | |
C18 | 0.6106 (6) | 1.1510 (5) | 0.3542 (2) | 0.0407 (15) | |
C19 | 0.7750 (7) | 1.0437 (7) | 0.4702 (2) | 0.070 (2) | |
H19A | 0.8559 | 1.0116 | 0.4518 | 0.105* | |
H19B | 0.7279 | 0.9742 | 0.4879 | 0.105* | |
H19C | 0.8031 | 1.1058 | 0.4929 | 0.105* | |
C20 | 0.6336 (6) | 1.1462 (6) | 0.2990 (2) | 0.0566 (17) | |
H20A | 0.5553 | 1.1844 | 0.2842 | 0.085* | |
H20B | 0.6431 | 1.0587 | 0.2894 | 0.085* | |
H20C | 0.7170 | 1.1925 | 0.2885 | 0.085* | |
C21 | 0.9967 (6) | 1.1994 (6) | 0.2865 (2) | 0.064 (2) | |
H21A | 1.0406 | 1.2816 | 0.2881 | 0.096* | |
H21B | 0.9040 | 1.2104 | 0.2759 | 0.096* | |
H21C | 1.0501 | 1.1474 | 0.2636 | 0.096* | |
C22 | 1.0357 (7) | 1.2420 (6) | 0.3927 (2) | 0.065 (2) | |
H22A | 1.0743 | 1.3158 | 0.3751 | 0.098* | |
H22B | 1.1035 | 1.2066 | 0.4134 | 0.098* | |
H22C | 0.9538 | 1.2665 | 0.4123 | 0.098* | |
C23 | 1.1972 (7) | 0.9651 (6) | 0.3033 (3) | 0.079 (2) | |
H23A | 1.2501 | 0.8886 | 0.3088 | 0.118* | |
H23B | 1.2596 | 1.0366 | 0.2982 | 0.118* | |
H23C | 1.1450 | 0.9555 | 0.2748 | 0.118* | |
C24 | 1.1655 (6) | 0.9534 (6) | 0.3908 (3) | 0.066 (2) | |
H24A | 1.2235 | 0.8795 | 0.3851 | 0.099* | |
H24B | 1.0953 | 0.9343 | 0.4166 | 0.099* | |
H24C | 1.2218 | 1.0235 | 0.4001 | 0.099* | |
N1 | 0.9057 (4) | 0.6959 (4) | 0.37359 (15) | 0.0332 (11) | |
N2 | 0.6412 (4) | 0.7597 (4) | 0.36734 (16) | 0.0398 (12) | |
N3 | 0.8352 (4) | 1.0458 (4) | 0.36536 (15) | 0.0322 (11) | |
N4 | 1.0997 (5) | 0.9877 (4) | 0.34669 (18) | 0.0447 (12) | |
Si1 | 0.74471 (17) | 0.62499 (15) | 0.37901 (6) | 0.0430 (4) | |
Si2 | 0.98807 (16) | 1.11987 (14) | 0.34818 (6) | 0.0385 (4) | |
Zn1 | 0.86701 (7) | 0.86979 (6) | 0.36550 (2) | 0.0404 (2) | |
C25 | 0.8211 (5) | 0.8591 (5) | 0.1183 (2) | 0.0347 (13) | |
C26 | 0.8934 (6) | 0.9011 (5) | 0.1581 (2) | 0.0410 (15) | |
C27 | 1.0259 (6) | 0.9538 (5) | 0.1489 (3) | 0.0514 (17) | |
H27A | 1.0741 | 0.9815 | 0.1751 | 0.062* | |
C28 | 1.0869 (7) | 0.9657 (5) | 0.1023 (3) | 0.061 (2) | |
H28A | 1.1746 | 1.0029 | 0.0969 | 0.073* | |
C29 | 1.0176 (6) | 0.9223 (5) | 0.0639 (3) | 0.0554 (18) | |
H29A | 1.0600 | 0.9288 | 0.0323 | 0.066* | |
C30 | 0.8862 (6) | 0.8690 (5) | 0.0708 (2) | 0.0388 (14) | |
C31 | 0.8312 (6) | 0.8870 (6) | 0.2093 (2) | 0.0610 (19) | |
H31A | 0.8950 | 0.9197 | 0.2315 | 0.091* | |
H31B | 0.8133 | 0.7981 | 0.2169 | 0.091* | |
H31C | 0.7452 | 0.9341 | 0.2125 | 0.091* | |
C32 | 0.8160 (6) | 0.8165 (6) | 0.0280 (2) | 0.0593 (18) | |
H32A | 0.7262 | 0.7827 | 0.0390 | 0.089* | |
H32B | 0.8725 | 0.7495 | 0.0135 | 0.089* | |
H32C | 0.8047 | 0.8837 | 0.0040 | 0.089* | |
C33 | 0.5070 (6) | 0.9918 (6) | 0.0798 (3) | 0.066 (2) | |
H33A | 0.4639 | 1.0680 | 0.0927 | 0.099* | |
H33B | 0.4493 | 0.9558 | 0.0563 | 0.099* | |
H33C | 0.5969 | 1.0126 | 0.0642 | 0.099* | |
C34 | 0.4760 (6) | 0.9561 (6) | 0.1889 (2) | 0.070 (2) | |
H34A | 0.4386 | 1.0393 | 0.1818 | 0.105* | |
H34B | 0.5563 | 0.9651 | 0.2077 | 0.105* | |
H34C | 0.4065 | 0.9059 | 0.2075 | 0.105* | |
C35 | 0.3731 (7) | 0.7072 (6) | 0.0787 (2) | 0.0622 (19) | |
H35A | 0.2835 | 0.7466 | 0.0757 | 0.093* | |
H35B | 0.3644 | 0.6161 | 0.0761 | 0.093* | |
H35C | 0.4376 | 0.7394 | 0.0530 | 0.093* | |
C36 | 0.3194 (6) | 0.7024 (6) | 0.1662 (2) | 0.064 (2) | |
H36A | 0.2368 | 0.7529 | 0.1628 | 0.096* | |
H36B | 0.3559 | 0.7183 | 0.1974 | 0.096* | |
H36C | 0.2967 | 0.6133 | 0.1644 | 0.096* | |
C37 | 0.4909 (5) | 0.3918 (5) | 0.13763 (19) | 0.0317 (13) | |
C38 | 0.4016 (6) | 0.3444 (5) | 0.1037 (2) | 0.0405 (15) | |
C39 | 0.2770 (6) | 0.2864 (5) | 0.1205 (2) | 0.0486 (16) | |
H39A | 0.2181 | 0.2545 | 0.0980 | 0.058* | |
C40 | 0.2395 (6) | 0.2756 (5) | 0.1696 (3) | 0.0531 (18) | |
H40A | 0.1565 | 0.2349 | 0.1802 | 0.064* | |
C41 | 0.3232 (6) | 0.3240 (5) | 0.2029 (2) | 0.0495 (17) | |
H41A | 0.2960 | 0.3179 | 0.2361 | 0.059* | |
C42 | 0.4501 (5) | 0.3829 (5) | 0.1873 (2) | 0.0380 (14) | |
C43 | 0.4373 (6) | 0.3560 (6) | 0.0493 (2) | 0.0563 (18) | |
H43A | 0.5258 | 0.3981 | 0.0433 | 0.084* | |
H43B | 0.3665 | 0.4052 | 0.0342 | 0.084* | |
H43C | 0.4424 | 0.2722 | 0.0356 | 0.084* | |
C44 | 0.5376 (6) | 0.4409 (6) | 0.2248 (2) | 0.0510 (16) | |
H44A | 0.6198 | 0.4787 | 0.2085 | 0.076* | |
H44B | 0.5643 | 0.3754 | 0.2475 | 0.076* | |
H44C | 0.4845 | 0.5056 | 0.2421 | 0.076* | |
C45 | 0.8064 (7) | 0.3256 (6) | 0.0441 (2) | 0.073 (2) | |
H45A | 0.8503 | 0.2429 | 0.0445 | 0.110* | |
H45B | 0.8659 | 0.3852 | 0.0254 | 0.110* | |
H45C | 0.7187 | 0.3196 | 0.0294 | 0.110* | |
C46 | 0.8057 (6) | 0.2434 (5) | 0.1506 (3) | 0.068 (2) | |
H46A | 0.8533 | 0.1766 | 0.1327 | 0.102* | |
H46B | 0.7175 | 0.2121 | 0.1646 | 0.102* | |
H46C | 0.8616 | 0.2701 | 0.1764 | 0.102* | |
C47 | 1.0029 (6) | 0.5425 (6) | 0.0775 (2) | 0.0612 (19) | |
H47A | 1.0530 | 0.6156 | 0.0877 | 0.092* | |
H47B | 0.9645 | 0.5619 | 0.0466 | 0.092* | |
H47C | 1.0655 | 0.4710 | 0.0739 | 0.092* | |
C48 | 0.9316 (6) | 0.5383 (6) | 0.1637 (2) | 0.0577 (18) | |
H48A | 0.9926 | 0.6112 | 0.1617 | 0.087* | |
H48B | 0.9801 | 0.4656 | 0.1765 | 0.087* | |
H48C | 0.8509 | 0.5564 | 0.1851 | 0.087* | |
N5 | 0.6876 (4) | 0.8031 (4) | 0.12634 (15) | 0.0322 (11) | |
N6 | 0.4247 (4) | 0.7370 (4) | 0.12669 (17) | 0.0382 (12) | |
N7 | 0.6194 (4) | 0.4531 (4) | 0.12183 (15) | 0.0297 (10) | |
N8 | 0.8880 (5) | 0.5102 (4) | 0.11487 (17) | 0.0423 (12) | |
Si3 | 0.52800 (16) | 0.87462 (14) | 0.13026 (6) | 0.0385 (4) | |
Si4 | 0.77609 (16) | 0.38238 (14) | 0.10839 (6) | 0.0372 (4) | |
Zn2 | 0.64533 (7) | 0.62880 (6) | 0.12387 (2) | 0.0391 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.031 (3) | 0.022 (3) | 0.048 (4) | 0.002 (2) | −0.001 (3) | −0.001 (3) |
C2 | 0.039 (4) | 0.027 (3) | 0.059 (4) | 0.001 (3) | 0.004 (3) | −0.008 (3) |
C3 | 0.044 (5) | 0.043 (4) | 0.103 (6) | −0.001 (3) | 0.026 (4) | −0.020 (4) |
C4 | 0.032 (4) | 0.032 (4) | 0.137 (8) | −0.001 (3) | −0.006 (5) | 0.002 (5) |
C5 | 0.045 (4) | 0.039 (4) | 0.090 (5) | −0.009 (3) | −0.026 (4) | 0.012 (4) |
C6 | 0.036 (4) | 0.029 (3) | 0.061 (4) | −0.006 (3) | −0.014 (3) | 0.006 (3) |
C7 | 0.076 (5) | 0.077 (5) | 0.056 (5) | −0.006 (4) | 0.026 (4) | −0.017 (4) |
C8 | 0.070 (5) | 0.064 (5) | 0.054 (4) | −0.006 (4) | −0.012 (4) | −0.003 (4) |
C9 | 0.043 (5) | 0.055 (5) | 0.186 (9) | −0.003 (4) | −0.008 (5) | −0.058 (5) |
C10 | 0.067 (6) | 0.135 (8) | 0.127 (8) | −0.033 (5) | −0.007 (5) | 0.078 (6) |
C11 | 0.075 (5) | 0.060 (5) | 0.092 (6) | −0.005 (4) | −0.032 (4) | 0.018 (4) |
C12 | 0.057 (5) | 0.053 (4) | 0.121 (7) | −0.015 (4) | 0.049 (5) | −0.020 (4) |
C13 | 0.024 (3) | 0.028 (3) | 0.045 (4) | −0.003 (2) | 0.009 (3) | −0.001 (3) |
C14 | 0.047 (4) | 0.045 (4) | 0.058 (4) | −0.009 (3) | 0.018 (3) | −0.007 (3) |
C15 | 0.070 (5) | 0.068 (5) | 0.060 (5) | −0.009 (4) | 0.031 (4) | −0.026 (4) |
C16 | 0.043 (5) | 0.057 (5) | 0.113 (7) | −0.001 (4) | 0.032 (5) | −0.025 (5) |
C17 | 0.035 (4) | 0.037 (4) | 0.091 (5) | 0.000 (3) | 0.001 (4) | −0.008 (4) |
C18 | 0.040 (4) | 0.022 (3) | 0.060 (4) | −0.003 (3) | 0.009 (3) | −0.007 (3) |
C19 | 0.073 (5) | 0.094 (6) | 0.041 (4) | −0.013 (4) | 0.012 (4) | −0.012 (4) |
C20 | 0.053 (4) | 0.044 (4) | 0.073 (5) | 0.008 (3) | −0.003 (3) | −0.004 (3) |
C21 | 0.051 (4) | 0.056 (4) | 0.080 (5) | −0.006 (3) | 0.025 (4) | 0.014 (4) |
C22 | 0.061 (5) | 0.044 (4) | 0.089 (5) | −0.019 (3) | 0.011 (4) | −0.017 (4) |
C23 | 0.053 (5) | 0.074 (5) | 0.107 (6) | 0.010 (4) | 0.015 (4) | −0.029 (5) |
C24 | 0.048 (4) | 0.046 (4) | 0.105 (6) | −0.008 (3) | −0.012 (4) | −0.001 (4) |
N1 | 0.035 (3) | 0.022 (2) | 0.043 (3) | 0.003 (2) | −0.002 (2) | −0.002 (2) |
N2 | 0.030 (3) | 0.039 (3) | 0.050 (3) | −0.001 (2) | 0.004 (2) | −0.007 (2) |
N3 | 0.027 (3) | 0.030 (3) | 0.039 (3) | −0.001 (2) | 0.008 (2) | −0.001 (2) |
N4 | 0.034 (3) | 0.042 (3) | 0.057 (3) | 0.007 (2) | −0.001 (2) | −0.007 (3) |
Si1 | 0.0330 (10) | 0.0317 (9) | 0.0642 (12) | −0.0015 (7) | −0.0019 (8) | 0.0012 (8) |
Si2 | 0.0325 (10) | 0.0299 (9) | 0.0517 (10) | −0.0044 (7) | 0.0087 (8) | −0.0028 (8) |
Zn1 | 0.0476 (5) | 0.0279 (4) | 0.0448 (4) | 0.0057 (3) | 0.0042 (3) | −0.0049 (3) |
C25 | 0.030 (3) | 0.017 (3) | 0.058 (4) | −0.002 (2) | −0.003 (3) | −0.004 (3) |
C26 | 0.028 (3) | 0.024 (3) | 0.072 (4) | 0.006 (3) | −0.009 (3) | −0.010 (3) |
C27 | 0.033 (4) | 0.036 (4) | 0.089 (5) | 0.006 (3) | −0.023 (4) | −0.018 (3) |
C28 | 0.040 (4) | 0.021 (3) | 0.121 (7) | −0.006 (3) | 0.002 (4) | −0.006 (4) |
C29 | 0.040 (4) | 0.033 (4) | 0.090 (5) | −0.004 (3) | 0.014 (4) | 0.006 (4) |
C30 | 0.031 (3) | 0.028 (3) | 0.056 (4) | −0.002 (3) | 0.004 (3) | 0.000 (3) |
C31 | 0.049 (4) | 0.069 (5) | 0.066 (5) | 0.006 (3) | −0.004 (3) | −0.026 (4) |
C32 | 0.050 (4) | 0.075 (5) | 0.050 (4) | 0.002 (3) | 0.013 (3) | −0.006 (4) |
C33 | 0.040 (4) | 0.049 (4) | 0.108 (6) | 0.006 (3) | 0.004 (4) | 0.016 (4) |
C34 | 0.052 (5) | 0.069 (5) | 0.088 (5) | 0.006 (4) | 0.008 (4) | −0.046 (4) |
C35 | 0.061 (5) | 0.046 (4) | 0.081 (5) | −0.002 (3) | −0.013 (4) | −0.014 (4) |
C36 | 0.054 (4) | 0.046 (4) | 0.086 (5) | 0.000 (3) | 0.031 (4) | 0.006 (4) |
C37 | 0.025 (3) | 0.023 (3) | 0.047 (3) | 0.002 (2) | 0.006 (3) | −0.001 (3) |
C38 | 0.032 (4) | 0.028 (3) | 0.060 (4) | −0.003 (3) | 0.003 (3) | 0.002 (3) |
C39 | 0.042 (4) | 0.031 (3) | 0.074 (5) | −0.007 (3) | −0.007 (3) | −0.009 (3) |
C40 | 0.032 (4) | 0.037 (4) | 0.087 (5) | −0.008 (3) | 0.020 (4) | 0.002 (4) |
C41 | 0.046 (4) | 0.041 (4) | 0.059 (4) | −0.006 (3) | 0.020 (3) | −0.004 (3) |
C42 | 0.030 (3) | 0.033 (3) | 0.050 (4) | −0.001 (3) | 0.007 (3) | 0.000 (3) |
C43 | 0.059 (4) | 0.052 (4) | 0.057 (4) | −0.013 (3) | −0.001 (3) | −0.011 (3) |
C44 | 0.052 (4) | 0.054 (4) | 0.044 (4) | −0.002 (3) | 0.013 (3) | −0.002 (3) |
C45 | 0.053 (5) | 0.077 (5) | 0.089 (5) | −0.010 (4) | 0.022 (4) | −0.045 (4) |
C46 | 0.050 (4) | 0.039 (4) | 0.114 (6) | 0.003 (3) | −0.003 (4) | 0.008 (4) |
C47 | 0.045 (4) | 0.055 (4) | 0.081 (5) | −0.008 (3) | 0.014 (4) | 0.003 (4) |
C48 | 0.045 (4) | 0.044 (4) | 0.084 (5) | −0.003 (3) | −0.004 (4) | −0.012 (4) |
N5 | 0.023 (3) | 0.026 (2) | 0.047 (3) | −0.0041 (19) | 0.002 (2) | −0.013 (2) |
N6 | 0.026 (3) | 0.032 (3) | 0.056 (3) | −0.002 (2) | 0.011 (2) | −0.003 (2) |
N7 | 0.023 (2) | 0.025 (2) | 0.040 (3) | −0.0024 (19) | 0.0054 (19) | −0.007 (2) |
N8 | 0.034 (3) | 0.039 (3) | 0.052 (3) | −0.008 (2) | 0.012 (2) | −0.008 (2) |
Si3 | 0.0314 (10) | 0.0260 (9) | 0.0575 (11) | 0.0003 (7) | 0.0042 (8) | −0.0088 (8) |
Si4 | 0.0317 (10) | 0.0265 (9) | 0.0526 (10) | −0.0008 (7) | 0.0054 (7) | −0.0075 (7) |
Zn2 | 0.0448 (5) | 0.0255 (4) | 0.0462 (4) | −0.0073 (3) | 0.0047 (3) | −0.0049 (3) |
C1—N1 | 1.389 (6) | C25—C26 | 1.408 (7) |
C1—C6 | 1.403 (7) | C25—N5 | 1.411 (6) |
C1—C2 | 1.426 (7) | C26—C27 | 1.391 (7) |
C2—C3 | 1.393 (8) | C26—C31 | 1.490 (8) |
C2—C7 | 1.471 (8) | C27—C28 | 1.369 (9) |
C3—C4 | 1.350 (9) | C27—H27A | 0.9300 |
C3—H3A | 0.9300 | C28—C29 | 1.368 (9) |
C4—C5 | 1.371 (9) | C28—H28A | 0.9300 |
C4—H4A | 0.9300 | C29—C30 | 1.380 (7) |
C5—C6 | 1.389 (8) | C29—H29A | 0.9300 |
C5—H5A | 0.9300 | C30—C32 | 1.505 (8) |
C6—C8 | 1.512 (8) | C31—H31A | 0.9600 |
C7—H7A | 0.9600 | C31—H31B | 0.9600 |
C7—H7B | 0.9600 | C31—H31C | 0.9600 |
C7—H7C | 0.9600 | C32—H32A | 0.9600 |
C8—H8A | 0.9600 | C32—H32B | 0.9600 |
C8—H8B | 0.9600 | C32—H32C | 0.9600 |
C8—H8C | 0.9600 | C33—Si3 | 1.843 (6) |
C9—Si1 | 1.864 (6) | C33—H33A | 0.9600 |
C9—H9A | 0.9600 | C33—H33B | 0.9600 |
C9—H9B | 0.9600 | C33—H33C | 0.9600 |
C9—H9C | 0.9600 | C34—Si3 | 1.871 (6) |
C10—Si1 | 1.862 (7) | C34—H34A | 0.9600 |
C10—H10A | 0.9600 | C34—H34B | 0.9600 |
C10—H10B | 0.9600 | C34—H34C | 0.9600 |
C10—H10C | 0.9600 | C35—N6 | 1.474 (7) |
C11—N2 | 1.449 (7) | C35—H35A | 0.9600 |
C11—H11A | 0.9600 | C35—H35B | 0.9600 |
C11—H11B | 0.9600 | C35—H35C | 0.9600 |
C11—H11C | 0.9600 | C36—N6 | 1.469 (6) |
C12—N2 | 1.469 (7) | C36—H36A | 0.9600 |
C12—H12A | 0.9600 | C36—H36B | 0.9600 |
C12—H12B | 0.9600 | C36—H36C | 0.9600 |
C12—H12C | 0.9600 | C37—C42 | 1.390 (7) |
C13—C18 | 1.393 (8) | C37—C38 | 1.404 (7) |
C13—C14 | 1.404 (8) | C37—N7 | 1.428 (6) |
C13—N3 | 1.422 (6) | C38—C39 | 1.387 (7) |
C14—C15 | 1.385 (8) | C38—C43 | 1.507 (7) |
C14—C19 | 1.495 (9) | C39—C40 | 1.368 (8) |
C15—C16 | 1.360 (10) | C39—H39A | 0.9300 |
C15—H15A | 0.9300 | C40—C41 | 1.360 (8) |
C16—C17 | 1.372 (9) | C40—H40A | 0.9300 |
C16—H16A | 0.9300 | C41—C42 | 1.402 (7) |
C17—C18 | 1.385 (7) | C41—H41A | 0.9300 |
C17—H17A | 0.9300 | C42—C44 | 1.505 (7) |
C18—C20 | 1.511 (8) | C43—H43A | 0.9600 |
C19—H19A | 0.9600 | C43—H43B | 0.9600 |
C19—H19B | 0.9600 | C43—H43C | 0.9600 |
C19—H19C | 0.9600 | C44—H44A | 0.9600 |
C20—H20A | 0.9600 | C44—H44B | 0.9600 |
C20—H20B | 0.9600 | C44—H44C | 0.9600 |
C20—H20C | 0.9600 | C45—Si4 | 1.872 (6) |
C21—Si2 | 1.860 (6) | C45—H45A | 0.9600 |
C21—H21A | 0.9600 | C45—H45B | 0.9600 |
C21—H21B | 0.9600 | C45—H45C | 0.9600 |
C21—H21C | 0.9600 | C46—Si4 | 1.867 (6) |
C22—Si2 | 1.862 (6) | C46—H46A | 0.9600 |
C22—H22A | 0.9600 | C46—H46B | 0.9600 |
C22—H22B | 0.9600 | C46—H46C | 0.9600 |
C22—H22C | 0.9600 | C47—N8 | 1.487 (6) |
C23—N4 | 1.485 (7) | C47—H47A | 0.9600 |
C23—H23A | 0.9600 | C47—H47B | 0.9600 |
C23—H23B | 0.9600 | C47—H47C | 0.9600 |
C23—H23C | 0.9600 | C48—N8 | 1.463 (7) |
C24—N4 | 1.435 (7) | C48—H48A | 0.9600 |
C24—H24A | 0.9600 | C48—H48B | 0.9600 |
C24—H24B | 0.9600 | C48—H48C | 0.9600 |
C24—H24C | 0.9600 | N5—Si3 | 1.701 (4) |
N1—Si1 | 1.712 (4) | N5—Zn2 | 1.871 (4) |
N1—Zn1 | 1.865 (4) | N6—Si3 | 1.757 (4) |
N2—Si1 | 1.756 (5) | N6—Zn2 | 2.396 (4) |
N2—Zn1 | 2.454 (4) | N7—Si4 | 1.696 (4) |
N3—Si2 | 1.694 (4) | N7—Zn2 | 1.856 (4) |
N3—Zn1 | 1.863 (4) | N8—Si4 | 1.735 (4) |
N4—Si2 | 1.745 (5) | Si3—Zn2 | 2.806 (2) |
C25—C30 | 1.404 (7) | Si4—Zn2 | 2.889 (2) |
N1—C1—C6 | 121.2 (5) | C26—C25—N5 | 120.4 (5) |
N1—C1—C2 | 120.4 (5) | C27—C26—C25 | 119.0 (6) |
C6—C1—C2 | 118.3 (5) | C27—C26—C31 | 120.2 (6) |
C3—C2—C1 | 117.9 (6) | C25—C26—C31 | 120.8 (5) |
C3—C2—C7 | 121.6 (6) | C28—C27—C26 | 121.5 (6) |
C1—C2—C7 | 120.5 (5) | C28—C27—H27A | 119.2 |
C4—C3—C2 | 122.9 (7) | C26—C27—H27A | 119.2 |
C4—C3—H3A | 118.5 | C29—C28—C27 | 119.4 (6) |
C2—C3—H3A | 118.5 | C29—C28—H28A | 120.3 |
C3—C4—C5 | 119.8 (7) | C27—C28—H28A | 120.3 |
C3—C4—H4A | 120.1 | C28—C29—C30 | 121.5 (6) |
C5—C4—H4A | 120.1 | C28—C29—H29A | 119.2 |
C4—C5—C6 | 120.3 (7) | C30—C29—H29A | 119.2 |
C4—C5—H5A | 119.8 | C29—C30—C25 | 119.7 (6) |
C6—C5—H5A | 119.8 | C29—C30—C32 | 120.0 (5) |
C5—C6—C1 | 120.7 (6) | C25—C30—C32 | 120.3 (5) |
C5—C6—C8 | 118.4 (6) | C26—C31—H31A | 109.5 |
C1—C6—C8 | 120.8 (5) | C26—C31—H31B | 109.5 |
C2—C7—H7A | 109.5 | H31A—C31—H31B | 109.5 |
C2—C7—H7B | 109.5 | C26—C31—H31C | 109.5 |
H7A—C7—H7B | 109.5 | H31A—C31—H31C | 109.5 |
C2—C7—H7C | 109.5 | H31B—C31—H31C | 109.5 |
H7A—C7—H7C | 109.5 | C30—C32—H32A | 109.5 |
H7B—C7—H7C | 109.5 | C30—C32—H32B | 109.5 |
C6—C8—H8A | 109.5 | H32A—C32—H32B | 109.5 |
C6—C8—H8B | 109.5 | C30—C32—H32C | 109.5 |
H8A—C8—H8B | 109.5 | H32A—C32—H32C | 109.5 |
C6—C8—H8C | 109.5 | H32B—C32—H32C | 109.5 |
H8A—C8—H8C | 109.5 | Si3—C33—H33A | 109.5 |
H8B—C8—H8C | 109.5 | Si3—C33—H33B | 109.5 |
Si1—C9—H9A | 109.5 | H33A—C33—H33B | 109.5 |
Si1—C9—H9B | 109.5 | Si3—C33—H33C | 109.5 |
H9A—C9—H9B | 109.5 | H33A—C33—H33C | 109.5 |
Si1—C9—H9C | 109.5 | H33B—C33—H33C | 109.5 |
H9A—C9—H9C | 109.5 | Si3—C34—H34A | 109.5 |
H9B—C9—H9C | 109.5 | Si3—C34—H34B | 109.5 |
Si1—C10—H10A | 109.5 | H34A—C34—H34B | 109.5 |
Si1—C10—H10B | 109.5 | Si3—C34—H34C | 109.5 |
H10A—C10—H10B | 109.5 | H34A—C34—H34C | 109.5 |
Si1—C10—H10C | 109.5 | H34B—C34—H34C | 109.5 |
H10A—C10—H10C | 109.5 | N6—C35—H35A | 109.5 |
H10B—C10—H10C | 109.5 | N6—C35—H35B | 109.5 |
N2—C11—H11A | 109.5 | H35A—C35—H35B | 109.5 |
N2—C11—H11B | 109.5 | N6—C35—H35C | 109.5 |
H11A—C11—H11B | 109.5 | H35A—C35—H35C | 109.5 |
N2—C11—H11C | 109.5 | H35B—C35—H35C | 109.5 |
H11A—C11—H11C | 109.5 | N6—C36—H36A | 109.5 |
H11B—C11—H11C | 109.5 | N6—C36—H36B | 109.5 |
N2—C12—H12A | 109.5 | H36A—C36—H36B | 109.5 |
N2—C12—H12B | 109.5 | N6—C36—H36C | 109.5 |
H12A—C12—H12B | 109.5 | H36A—C36—H36C | 109.5 |
N2—C12—H12C | 109.5 | H36B—C36—H36C | 109.5 |
H12A—C12—H12C | 109.5 | C42—C37—C38 | 119.0 (5) |
H12B—C12—H12C | 109.5 | C42—C37—N7 | 119.8 (5) |
C18—C13—C14 | 118.5 (5) | C38—C37—N7 | 121.2 (5) |
C18—C13—N3 | 121.1 (5) | C39—C38—C37 | 119.5 (5) |
C14—C13—N3 | 120.4 (5) | C39—C38—C43 | 119.0 (5) |
C15—C14—C13 | 118.8 (6) | C37—C38—C43 | 121.5 (5) |
C15—C14—C19 | 120.6 (6) | C40—C39—C38 | 120.9 (6) |
C13—C14—C19 | 120.5 (5) | C40—C39—H39A | 119.5 |
C16—C15—C14 | 122.7 (7) | C38—C39—H39A | 119.5 |
C16—C15—H15A | 118.7 | C41—C40—C39 | 120.3 (5) |
C14—C15—H15A | 118.7 | C41—C40—H40A | 119.9 |
C15—C16—C17 | 118.6 (6) | C39—C40—H40A | 119.9 |
C15—C16—H16A | 120.7 | C40—C41—C42 | 120.4 (6) |
C17—C16—H16A | 120.7 | C40—C41—H41A | 119.8 |
C16—C17—C18 | 121.0 (7) | C42—C41—H41A | 119.8 |
C16—C17—H17A | 119.5 | C37—C42—C41 | 119.8 (5) |
C18—C17—H17A | 119.5 | C37—C42—C44 | 120.8 (5) |
C17—C18—C13 | 120.4 (6) | C41—C42—C44 | 119.3 (5) |
C17—C18—C20 | 118.2 (6) | C38—C43—H43A | 109.5 |
C13—C18—C20 | 121.4 (5) | C38—C43—H43B | 109.5 |
C14—C19—H19A | 109.5 | H43A—C43—H43B | 109.5 |
C14—C19—H19B | 109.5 | C38—C43—H43C | 109.5 |
H19A—C19—H19B | 109.5 | H43A—C43—H43C | 109.5 |
C14—C19—H19C | 109.5 | H43B—C43—H43C | 109.5 |
H19A—C19—H19C | 109.5 | C42—C44—H44A | 109.5 |
H19B—C19—H19C | 109.5 | C42—C44—H44B | 109.5 |
C18—C20—H20A | 109.5 | H44A—C44—H44B | 109.5 |
C18—C20—H20B | 109.5 | C42—C44—H44C | 109.5 |
H20A—C20—H20B | 109.5 | H44A—C44—H44C | 109.5 |
C18—C20—H20C | 109.5 | H44B—C44—H44C | 109.5 |
H20A—C20—H20C | 109.5 | Si4—C45—H45A | 109.5 |
H20B—C20—H20C | 109.5 | Si4—C45—H45B | 109.5 |
Si2—C21—H21A | 109.5 | H45A—C45—H45B | 109.5 |
Si2—C21—H21B | 109.5 | Si4—C45—H45C | 109.5 |
H21A—C21—H21B | 109.5 | H45A—C45—H45C | 109.5 |
Si2—C21—H21C | 109.5 | H45B—C45—H45C | 109.5 |
H21A—C21—H21C | 109.5 | Si4—C46—H46A | 109.5 |
H21B—C21—H21C | 109.5 | Si4—C46—H46B | 109.5 |
Si2—C22—H22A | 109.5 | H46A—C46—H46B | 109.5 |
Si2—C22—H22B | 109.5 | Si4—C46—H46C | 109.5 |
H22A—C22—H22B | 109.5 | H46A—C46—H46C | 109.5 |
Si2—C22—H22C | 109.5 | H46B—C46—H46C | 109.5 |
H22A—C22—H22C | 109.5 | N8—C47—H47A | 109.5 |
H22B—C22—H22C | 109.5 | N8—C47—H47B | 109.5 |
N4—C23—H23A | 109.5 | H47A—C47—H47B | 109.5 |
N4—C23—H23B | 109.5 | N8—C47—H47C | 109.5 |
H23A—C23—H23B | 109.5 | H47A—C47—H47C | 109.5 |
N4—C23—H23C | 109.5 | H47B—C47—H47C | 109.5 |
H23A—C23—H23C | 109.5 | N8—C48—H48A | 109.5 |
H23B—C23—H23C | 109.5 | N8—C48—H48B | 109.5 |
N4—C24—H24A | 109.5 | H48A—C48—H48B | 109.5 |
N4—C24—H24B | 109.5 | N8—C48—H48C | 109.5 |
H24A—C24—H24B | 109.5 | H48A—C48—H48C | 109.5 |
N4—C24—H24C | 109.5 | H48B—C48—H48C | 109.5 |
H24A—C24—H24C | 109.5 | C25—N5—Si3 | 129.3 (3) |
H24B—C24—H24C | 109.5 | C25—N5—Zn2 | 126.4 (3) |
C1—N1—Si1 | 127.7 (4) | Si3—N5—Zn2 | 103.5 (2) |
C1—N1—Zn1 | 128.2 (3) | C36—N6—C35 | 110.2 (5) |
Si1—N1—Zn1 | 104.2 (2) | C36—N6—Si3 | 120.8 (4) |
C11—N2—C12 | 111.4 (5) | C35—N6—Si3 | 117.8 (4) |
C11—N2—Si1 | 118.2 (4) | C36—N6—Zn2 | 118.6 (4) |
C12—N2—Si1 | 119.0 (4) | C35—N6—Zn2 | 102.2 (3) |
C11—N2—Zn1 | 108.7 (4) | Si3—N6—Zn2 | 83.50 (17) |
C12—N2—Zn1 | 113.3 (3) | C37—N7—Si4 | 127.4 (3) |
Si1—N2—Zn1 | 82.41 (17) | C37—N7—Zn2 | 123.0 (3) |
C13—N3—Si2 | 128.7 (3) | Si4—N7—Zn2 | 108.8 (2) |
C13—N3—Zn1 | 122.6 (3) | C48—N8—C47 | 109.6 (4) |
Si2—N3—Zn1 | 107.9 (2) | C48—N8—Si4 | 118.9 (4) |
C24—N4—C23 | 109.9 (5) | C47—N8—Si4 | 122.0 (4) |
C24—N4—Si2 | 117.7 (4) | N5—Si3—N6 | 98.4 (2) |
C23—N4—Si2 | 120.8 (4) | N5—Si3—C33 | 112.3 (2) |
N1—Si1—N2 | 99.1 (2) | N6—Si3—C33 | 113.5 (3) |
N1—Si1—C10 | 115.3 (3) | N5—Si3—C34 | 116.7 (3) |
N2—Si1—C10 | 110.4 (3) | N6—Si3—C34 | 108.6 (3) |
N1—Si1—C9 | 113.4 (3) | C33—Si3—C34 | 107.3 (3) |
N2—Si1—C9 | 111.9 (3) | N5—Si3—Zn2 | 40.42 (13) |
C10—Si1—C9 | 106.6 (4) | N6—Si3—Zn2 | 58.04 (15) |
N3—Si2—N4 | 99.7 (2) | C33—Si3—Zn2 | 127.5 (2) |
N3—Si2—C21 | 115.4 (3) | C34—Si3—Zn2 | 124.8 (2) |
N4—Si2—C21 | 109.0 (3) | N7—Si4—N8 | 100.7 (2) |
N3—Si2—C22 | 112.5 (2) | N7—Si4—C46 | 111.7 (2) |
N4—Si2—C22 | 113.1 (3) | N8—Si4—C46 | 113.9 (3) |
C21—Si2—C22 | 107.2 (3) | N7—Si4—C45 | 115.6 (3) |
N3—Si2—Zn1 | 38.03 (14) | N8—Si4—C45 | 107.4 (3) |
N4—Si2—Zn1 | 61.91 (16) | C46—Si4—C45 | 107.6 (3) |
C21—Si2—Zn1 | 121.8 (2) | N7—Si4—Zn2 | 37.46 (13) |
C22—Si2—Zn1 | 129.9 (2) | N8—Si4—Zn2 | 63.91 (16) |
N3—Zn1—N1 | 172.83 (18) | C46—Si4—Zn2 | 132.3 (2) |
N3—Zn1—N2 | 108.62 (17) | C45—Si4—Zn2 | 118.6 (2) |
N1—Zn1—N2 | 73.96 (17) | N7—Zn2—N5 | 175.11 (18) |
N3—Zn1—Si1 | 145.60 (13) | N7—Zn2—N6 | 110.30 (16) |
N1—Zn1—Si1 | 36.01 (13) | N5—Zn2—N6 | 74.56 (16) |
N2—Zn1—Si1 | 38.08 (11) | N7—Zn2—Si3 | 148.71 (13) |
N3—Zn1—Si2 | 34.06 (12) | N5—Zn2—Si3 | 36.13 (13) |
N1—Zn1—Si2 | 144.76 (14) | N6—Zn2—Si3 | 38.46 (10) |
N2—Zn1—Si2 | 140.86 (11) | N7—Zn2—Si4 | 33.75 (12) |
Si1—Zn1—Si2 | 177.91 (6) | N5—Zn2—Si4 | 141.55 (13) |
C30—C25—C26 | 118.9 (5) | N6—Zn2—Si4 | 143.08 (11) |
C30—C25—N5 | 120.6 (5) | Si3—Zn2—Si4 | 174.78 (5) |
Experimental details
Crystal data | |
Chemical formula | [Zn(C12H21N2Si)2] |
Mr | 508.17 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 9.600 (5), 10.447 (5), 27.338 (5) |
α, β, γ (°) | 88.654 (5), 86.151 (5), 89.858 (5) |
V (Å3) | 2735 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.00 |
Crystal size (mm) | 0.25 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.788, 0.825 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11316, 9429, 5229 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.064, 0.161, 0.90 |
No. of reflections | 9429 |
No. of parameters | 559 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.83, −0.61 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL/PC (Sheldrick, 1999).
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Zinc amides were a class of transamination reagents (Amstrong et al., 2002). They were also useful in preparing the zinc thin film through the MOVCD method (Maile et al., 2005).
The title compound is monomeric, and is similar to bis[(N-trimethylsilyl)-2,6-dimethylanilido]zinc and bis[(N-dimethylaminodimethylsilyl)-2,6-diisopropylanilido]zinc (Schumann et al., 2000). The ligand has an N—Si—N chelating group, which is presumed to be a "quasi" conjugated unit owing to d–π interaction between Si and N atoms. The Zn center is chelated, with an average N—Zn—N bite angle of 74°. Compared with the rigid N—C—N chelating unit in the amidinate ligand, the N—Si—N group is much more flexible. The Zn—Nanilido bonds are in the normal range whereas the Zn—Namino bonds are more than 2.40 Å (Engelhardt et al., 1991). The linear N1—Zn1—N3 is nearly linear; this feature has also been observed in bis[(N-trimethylsilyl)-2,6-dimethylanilido]zinc. In the present compound, for both independent molecules, the two ligands are arranged in trans to each other. The [NZnN] planes are approximately coplanar. In the reported bis[(N-dimethylaminodimethylsilyl)-2,6-diisopropylanilido]zinc, the ligands are cis to each other in the tetrahedron around zinc. Evidently, the steric effect of the aromatic substituents plays an important role in influencing the geometry of zinc in this class of zinc amides.