Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768107045880/bs5050sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768107045880/bs5050sup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768107045880/bs5050sup3.pdf |
CCDC references: 637340; 637976
Data collection: CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) for znzn; LAUEGEN for zn-zn. Cell refinement: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) for znzn. Data reduction: CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05)
SORTAV (Blessing, 1989) for znzn; ARGONNE BOXES for zn-zn. Program(s) used to solve structure: SHELXS97 (Sheldrick, 1997) for znzn. Program(s) used to refine structure: XD2006 (Volkov et al., 2006) for znzn; SHELXL97 (Sheldrick, 1997) for zn-zn. Molecular graphics: XD2006 (Volkov et al., 2006) for znzn; SHELXTL for zn-zn. Software used to prepare material for publication: XD2006 (Volkov et al., 2006) for znzn; SHELXTL for zn-zn.
C20H30Zn2 | Z = 2 |
Mr = 401.18 | F(000) = 420 |
Triclinic, P1 | Dx = 1.399 Mg m−3 |
a = 6.9115 (6) Å | Synchrotron radiation, λ = 0.71000 Å |
b = 10.8895 (14) Å | Cell parameters from 5456 reflections |
c = 13.8927 (14) Å | θ = 3.0–29.3° |
α = 109.908 (10)° | µ = 2.51 mm−1 |
β = 101.551 (8)° | T = 100 K |
γ = 93.905 (9)° | Plate, colourless |
V = 952.61 (18) Å3 | 0.70 × 0.70 × 0.05 mm |
CCD area detector diffractometer | 12354 reflections with I > 2σ(I) |
Radiation source: ESRF BM01A | Rint = 0.054 |
phi and ω scans | θmax = 43.5°, θmin = 2.0° |
Absorption correction: multi-scan SADABS | h = −13→14 |
Tmin = 0.272, Tmax = 0.881 | k = −23→21 |
57003 measured reflections | l = 0→30 |
13873 independent reflections |
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.040 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.10 | w = 1/[σ2(Fo)] |
11249 reflections | (Δ/σ)max = 0.047 |
782 parameters | Δρmax = 0.59 e Å−3 |
0 restraints | Δρmin = −0.48 e Å−3 |
132 constraints |
C20H30Zn2 | γ = 93.905 (9)° |
Mr = 401.18 | V = 952.61 (18) Å3 |
Triclinic, P1 | Z = 2 |
a = 6.9115 (6) Å | Synchrotron radiation, λ = 0.71000 Å |
b = 10.8895 (14) Å | µ = 2.51 mm−1 |
c = 13.8927 (14) Å | T = 100 K |
α = 109.908 (10)° | 0.70 × 0.70 × 0.05 mm |
β = 101.551 (8)° |
CCD area detector diffractometer | 13873 independent reflections |
Absorption correction: multi-scan SADABS | 12354 reflections with I > 2σ(I) |
Tmin = 0.272, Tmax = 0.881 | Rint = 0.054 |
57003 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 0 restraints |
wR(F2) = 0.040 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.10 | Δρmax = 0.59 e Å−3 |
11249 reflections | Δρmin = −0.48 e Å−3 |
782 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
ZN(1) | 0.66367 (5) | 0.27955 (5) | 0.68212 (4) | 0.015 | |
ZN(2) | 0.85430 (5) | 0.20952 (6) | 0.80545 (5) | 0.015 | |
C(1) | 0.49605 (18) | 0.23498 (13) | 0.51129 (12) | 0.014 | |
C(2) | 0.63474 (17) | 0.35452 (15) | 0.54645 (13) | 0.016 | |
C(3) | 0.57612 (19) | 0.45008 (13) | 0.63106 (13) | 0.017 | |
C(4) | 0.39994 (19) | 0.39082 (14) | 0.64894 (13) | 0.016 | |
C(5) | 0.35141 (16) | 0.25743 (13) | 0.57420 (12) | 0.015 | |
C(6) | 1.02717 (19) | 0.05026 (14) | 0.83802 (13) | 0.016 | |
C(7) | 1.16296 (17) | 0.17117 (15) | 0.87361 (13) | 0.017 | |
C(8) | 1.09987 (19) | 0.26642 (14) | 0.95679 (13) | 0.018 | |
C(9) | 0.9244 (2) | 0.20495 (15) | 0.97326 (13) | 0.017 | |
C(10) | 0.88000 (18) | 0.07077 (14) | 0.89965 (12) | 0.016 | |
C(11) | 0.4919 (2) | 0.11218 (16) | 0.41860 (14) | 0.025 | |
C(12) | 0.79679 (19) | 0.38145 (19) | 0.49524 (15) | 0.028 | |
C(13) | 0.6709 (2) | 0.59243 (14) | 0.68411 (15) | 0.03 | |
C(14) | 0.2830 (3) | 0.4594 (2) | 0.72592 (16) | 0.026 | |
C(15) | 0.17041 (17) | 0.16067 (15) | 0.55781 (13) | 0.023 | |
C(16) | 1.0476 (3) | −0.07690 (18) | 0.75540 (17) | 0.027 | |
C(17) | 1.34887 (18) | 0.18959 (18) | 0.83661 (15) | 0.026 | |
C(18) | 1.2115 (3) | 0.40205 (16) | 1.02274 (15) | 0.031 | |
C(19) | 0.8207 (3) | 0.2665 (2) | 1.05834 (16) | 0.029 | |
C(20) | 0.72291 (18) | −0.03391 (15) | 0.89724 (13) | 0.023 | |
H(11A) | 0.615799 | 0.122606 | 0.387484 | 0.036* | |
H(11B) | 0.359902 | 0.096723 | 0.360643 | 0.036* | |
H(11C) | 0.496263 | 0.030938 | 0.442953 | 0.036* | |
H(12A) | 0.808365 | 0.294254 | 0.435193 | 0.047* | |
H(12B) | 0.93309 | 0.415286 | 0.551929 | 0.047* | |
H(12C) | 0.762135 | 0.45396 | 0.4632 | 0.047* | |
H(13A) | 0.60062 | 0.640921 | 0.743861 | 0.041* | |
H(13B) | 0.655698 | 0.638277 | 0.628229 | 0.041* | |
H(13C) | 0.823163 | 0.597377 | 0.716822 | 0.041* | |
H(14A) | 0.355469 | 0.556065 | 0.770214 | 0.04* | 0.1177 |
H(14B) | 0.271258 | 0.407687 | 0.776424 | 0.04* | 0.1177 |
H(14C) | 0.139601 | 0.462541 | 0.684809 | 0.04* | 0.1177 |
H(14D) | 0.155362 | 0.394965 | 0.717327 | 0.04* | 0.8823 |
H(14E) | 0.239379 | 0.542963 | 0.711146 | 0.04* | 0.8823 |
H(14F) | 0.371587 | 0.488364 | 0.802975 | 0.04* | 0.8823 |
H(15A) | 0.090395 | 0.202017 | 0.614771 | 0.036* | 0.6691 |
H(15B) | 0.215736 | 0.073625 | 0.565246 | 0.036* | 0.6691 |
H(15C) | 0.078582 | 0.138703 | 0.482333 | 0.036* | 0.6691 |
H(15D) | 0.166269 | 0.074058 | 0.493453 | 0.036* | 0.3309 |
H(15E) | 0.04069 | 0.202726 | 0.54314 | 0.036* | 0.3309 |
H(15F) | 0.177756 | 0.137559 | 0.625757 | 0.036* | 0.3309 |
H(16A) | 1.168312 | −0.061042 | 0.72358 | 0.041* | 0.2798 |
H(16B) | 0.91589 | −0.109842 | 0.695317 | 0.041* | 0.2798 |
H(16C) | 1.072093 | −0.14845 | 0.789716 | 0.041* | 0.2798 |
H(16D) | 0.935977 | −0.151708 | 0.748709 | 0.041* | 0.7202 |
H(16E) | 1.188607 | −0.103088 | 0.777237 | 0.041* | 0.7202 |
H(16F) | 1.03171 | −0.064534 | 0.682672 | 0.041* | 0.7202 |
H(17A) | 1.356705 | 0.103259 | 0.77469 | 0.044* | |
H(17B) | 1.47445 | 0.209474 | 0.899264 | 0.044* | |
H(17C) | 1.345351 | 0.269167 | 0.810229 | 0.044* | |
H(18A) | 1.132892 | 0.451856 | 1.077935 | 0.042* | |
H(18B) | 1.227138 | 0.455188 | 0.97365 | 0.042* | |
H(18C) | 1.35395 | 0.394376 | 1.062098 | 0.042* | |
H(19A) | 0.884839 | 0.365642 | 1.099382 | 0.047* | 0.2994 |
H(19B) | 0.835746 | 0.21584 | 1.110954 | 0.047* | 0.2994 |
H(19C) | 0.668637 | 0.261652 | 1.025194 | 0.047* | 0.2994 |
H(19D) | 0.708066 | 0.196342 | 1.057704 | 0.047* | 0.7006 |
H(19E) | 0.757211 | 0.346407 | 1.046096 | 0.047* | 0.7006 |
H(19F) | 0.923942 | 0.300389 | 1.131732 | 0.047* | 0.7006 |
H(20A) | 0.636039 | 0.008457 | 0.950368 | 0.038* | |
H(20B) | 0.791865 | −0.107285 | 0.917917 | 0.038* | |
H(20C) | 0.630656 | −0.076661 | 0.820856 | 0.038* |
U11 | U22 | U33 | U12 | U13 | U23 | |
ZN(1) | 0.01471 (11) | 0.01646 (12) | 0.01633 (14) | 0.00333 (12) | 0.00233 (13) | 0.01069 (14) |
ZN(2) | 0.01384 (10) | 0.01789 (12) | 0.01625 (14) | 0.00391 (12) | 0.00263 (12) | 0.01101 (14) |
C(1) | 0.0159 (4) | 0.0139 (4) | 0.0142 (5) | 0.0029 (3) | 0.0033 (4) | 0.0060 (4) |
C(2) | 0.0139 (3) | 0.0195 (5) | 0.0194 (5) | 0.0004 (4) | 0.0027 (4) | 0.0123 (5) |
C(3) | 0.0181 (4) | 0.0125 (4) | 0.0198 (6) | −0.0004 (3) | −0.0009 (4) | 0.0074 (5) |
C(4) | 0.0166 (4) | 0.0166 (5) | 0.0163 (6) | 0.0046 (4) | 0.0032 (4) | 0.0070 (5) |
C(5) | 0.0123 (3) | 0.0152 (4) | 0.0167 (5) | 0.0001 (3) | 0.0016 (4) | 0.0074 (4) |
C(6) | 0.0168 (4) | 0.0157 (5) | 0.0168 (6) | 0.0053 (4) | 0.0049 (4) | 0.0079 (5) |
C(7) | 0.0124 (3) | 0.0215 (5) | 0.0198 (6) | 0.0031 (4) | 0.0036 (4) | 0.0120 (5) |
C(8) | 0.0179 (4) | 0.0174 (5) | 0.0183 (6) | −0.0007 (4) | −0.0014 (4) | 0.0088 (5) |
C(9) | 0.0180 (4) | 0.0198 (5) | 0.0148 (5) | 0.0054 (4) | 0.0052 (4) | 0.0080 (5) |
C(10) | 0.0158 (4) | 0.0175 (5) | 0.0176 (5) | 0.0019 (4) | 0.0035 (4) | 0.0102 (5) |
C(11) | 0.0325 (6) | 0.0208 (5) | 0.0185 (7) | 0.0086 (5) | 0.0040 (6) | 0.0048 (6) |
C(12) | 0.0171 (4) | 0.0442 (8) | 0.0342 (8) | 0.0024 (5) | 0.0076 (5) | 0.0291 (8) |
C(13) | 0.0344 (6) | 0.0150 (5) | 0.0330 (8) | −0.0046 (5) | −0.0095 (6) | 0.0106 (6) |
C(14) | 0.0282 (6) | 0.0327 (7) | 0.0195 (7) | 0.0148 (6) | 0.0068 (6) | 0.0092 (7) |
C(15) | 0.0142 (3) | 0.0261 (6) | 0.0284 (7) | −0.0034 (4) | 0.0011 (4) | 0.0146 (6) |
C(16) | 0.0321 (6) | 0.0222 (6) | 0.0278 (8) | 0.0110 (6) | 0.0083 (7) | 0.0078 (7) |
C(17) | 0.0142 (4) | 0.0387 (8) | 0.0333 (8) | 0.0053 (5) | 0.0078 (5) | 0.0231 (7) |
C(18) | 0.0340 (6) | 0.0212 (6) | 0.0266 (8) | −0.0046 (5) | −0.0076 (6) | 0.0057 (6) |
C(19) | 0.0351 (7) | 0.0382 (9) | 0.0187 (7) | 0.0117 (7) | 0.0120 (6) | 0.0107 (8) |
C(20) | 0.0189 (4) | 0.0269 (6) | 0.0298 (7) | −0.0010 (4) | 0.0037 (5) | 0.0190 (6) |
ZN(1)—ZN(2) | 2.3186 (3) | C(14)—H(14C) | 1.0495 (14) |
C(1)—C(2) | 1.4358 (15) | C(14)—H(14D) | 1.0495 (19) |
C(1)—C(5) | 1.436 (2) | C(14)—H(14E) | 1.0495 (17) |
C(1)—C(11) | 1.502 (3) | C(14)—H(14F) | 1.0495 (15) |
C(2)—C(3) | 1.430 (3) | C(15)—H(15A) | 1.050 (2) |
C(2)—C(12) | 1.504 (2) | C(15)—H(15B) | 1.0495 (14) |
C(3)—C(4) | 1.444 (2) | C(15)—H(15C) | 1.0495 (12) |
C(3)—C(13) | 1.5051 (17) | C(15)—H(15D) | 1.0495 (19) |
C(4)—C(5) | 1.438 (2) | C(15)—H(15E) | 1.0495 (14) |
C(4)—C(14) | 1.496 (3) | C(15)—H(15F) | 1.0495 (14) |
C(5)—C(15) | 1.5066 (14) | C(16)—H(16A) | 1.049 (2) |
C(6)—C(7) | 1.4357 (16) | C(16)—H(16B) | 1.0495 (14) |
C(6)—C(10) | 1.438 (2) | C(16)—H(16C) | 1.0495 (15) |
C(6)—C(16) | 1.505 (3) | C(16)—H(16D) | 1.0495 (17) |
C(7)—C(8) | 1.431 (3) | C(16)—H(16E) | 1.0495 (17) |
C(7)—C(17) | 1.502 (2) | C(16)—H(16F) | 1.049 (2) |
C(8)—C(9) | 1.441 (2) | C(17)—H(17A) | 1.049 (2) |
C(8)—C(18) | 1.5022 (19) | C(17)—H(17B) | 1.0495 (11) |
C(9)—C(10) | 1.439 (2) | C(17)—H(17C) | 1.0495 (13) |
C(9)—C(19) | 1.492 (3) | C(18)—H(18A) | 1.050 (3) |
C(10)—C(20) | 1.5067 (16) | C(18)—H(18B) | 1.0495 (17) |
C(11)—H(11A) | 1.050 (2) | C(18)—H(18C) | 1.0495 (15) |
C(11)—H(11B) | 1.0495 (12) | C(19)—H(19A) | 1.049 (2) |
C(11)—H(11C) | 1.0495 (14) | C(19)—H(19B) | 1.0495 (17) |
C(12)—H(12A) | 1.050 (2) | C(19)—H(19C) | 1.0495 (19) |
C(12)—H(12B) | 1.0495 (12) | C(19)—H(19D) | 1.050 (2) |
C(12)—H(12C) | 1.0495 (13) | C(19)—H(19E) | 1.050 (2) |
C(13)—H(13A) | 1.049 (3) | C(19)—H(19F) | 1.0495 (16) |
C(13)—H(13B) | 1.0495 (15) | C(20)—H(20A) | 1.050 (2) |
C(13)—H(13C) | 1.0495 (14) | C(20)—H(20B) | 1.0495 (13) |
C(14)—H(14A) | 1.0495 (19) | C(20)—H(20C) | 1.0495 (14) |
C(14)—H(14B) | 1.0495 (18) | ||
C(2)—C(1)—C(5) | 108.04 (15) | H(15A)—C(15)—H(15B) | 109.19 (13) |
C(2)—C(1)—C(11) | 125.91 (17) | H(15A)—C(15)—H(15C) | 109.43 (11) |
C(5)—C(1)—C(11) | 125.83 (11) | H(15A)—C(15)—H(15D) | 140.86 (11) |
C(1)—C(2)—C(3) | 107.82 (14) | H(15A)—C(15)—H(15E) | 56.19 (9) |
C(1)—C(2)—C(12) | 126.44 (18) | H(15A)—C(15)—H(15F) | 56.10 (10) |
C(3)—C(2)—C(12) | 125.31 (13) | H(15B)—C(15)—H(15C) | 109.49 (15) |
C(2)—C(3)—C(4) | 108.63 (11) | H(15B)—C(15)—H(15D) | 56.24 (9) |
C(2)—C(3)—C(13) | 125.01 (15) | H(15B)—C(15)—H(15E) | 140.85 (11) |
C(4)—C(3)—C(13) | 126.07 (19) | H(15B)—C(15)—H(15F) | 56.12 (6) |
C(3)—C(4)—C(5) | 107.11 (16) | H(15C)—C(15)—H(15D) | 56.32 (9) |
C(3)—C(4)—C(14) | 125.91 (14) | H(15C)—C(15)—H(15E) | 56.30 (5) |
C(5)—C(4)—C(14) | 126.84 (13) | H(15C)—C(15)—H(15F) | 140.85 (11) |
C(1)—C(5)—C(4) | 108.39 (11) | H(15D)—C(15)—H(15E) | 109.55 (10) |
C(1)—C(5)—C(15) | 125.27 (15) | H(15D)—C(15)—H(15F) | 109.31 (12) |
C(4)—C(5)—C(15) | 126.16 (17) | H(15E)—C(15)—H(15F) | 109.25 (17) |
C(7)—C(6)—C(10) | 108.12 (16) | C(6)—C(16)—H(16A) | 109.47 (14) |
C(7)—C(6)—C(16) | 124.80 (17) | C(6)—C(16)—H(16B) | 109.40 (16) |
C(10)—C(6)—C(16) | 126.96 (12) | C(6)—C(16)—H(16C) | 109.41 (19) |
C(6)—C(7)—C(8) | 107.96 (14) | C(6)—C(16)—H(16D) | 109.4 (2) |
C(6)—C(7)—C(17) | 125.56 (18) | C(6)—C(16)—H(16E) | 109.45 (14) |
C(8)—C(7)—C(17) | 126.25 (13) | C(6)—C(16)—H(16F) | 109.44 (13) |
C(7)—C(8)—C(9) | 108.32 (12) | H(16A)—C(16)—H(16B) | 109.5 (2) |
C(7)—C(8)—C(18) | 125.23 (16) | H(16A)—C(16)—H(16C) | 109.73 (17) |
C(9)—C(8)—C(18) | 126.1 (2) | H(16A)—C(16)—H(16D) | 141.1 (2) |
C(8)—C(9)—C(10) | 107.62 (17) | H(16A)—C(16)—H(16E) | 56.41 (11) |
C(8)—C(9)—C(19) | 125.58 (16) | H(16A)—C(16)—H(16F) | 56.32 (12) |
C(10)—C(9)—C(19) | 126.56 (14) | H(16B)—C(16)—H(16C) | 109.34 (14) |
C(6)—C(10)—C(9) | 107.98 (11) | H(16B)—C(16)—H(16D) | 56.12 (8) |
C(6)—C(10)—C(20) | 125.98 (15) | H(16B)—C(16)—H(16E) | 141.1 (2) |
C(9)—C(10)—C(20) | 125.63 (17) | H(16B)—C(16)—H(16F) | 56.17 (9) |
C(1)—C(11)—H(11A) | 109.64 (12) | H(16C)—C(16)—H(16D) | 56.21 (8) |
C(1)—C(11)—H(11B) | 109.43 (16) | H(16C)—C(16)—H(16E) | 56.36 (8) |
C(1)—C(11)—H(11C) | 109.40 (15) | H(16C)—C(16)—H(16F) | 141.1 (2) |
H(11A)—C(11)—H(11B) | 109.63 (17) | H(16D)—C(16)—H(16E) | 109.55 (14) |
H(11A)—C(11)—H(11C) | 109.53 (17) | H(16D)—C(16)—H(16F) | 109.31 (14) |
H(11B)—C(11)—H(11C) | 109.20 (13) | H(16E)—C(16)—H(16F) | 109.7 (2) |
C(2)—C(12)—H(12A) | 109.51 (12) | C(7)—C(17)—H(17A) | 109.49 (12) |
C(2)—C(12)—H(12B) | 109.39 (14) | C(7)—C(17)—H(17B) | 109.43 (15) |
C(2)—C(12)—H(12C) | 109.46 (15) | C(7)—C(17)—H(17C) | 109.42 (14) |
H(12A)—C(12)—H(12B) | 109.55 (16) | H(17A)—C(17)—H(17B) | 109.54 (15) |
H(12A)—C(12)—H(12C) | 109.62 (16) | H(17A)—C(17)—H(17C) | 109.58 (17) |
H(12B)—C(12)—H(12C) | 109.30 (13) | H(17B)—C(17)—H(17C) | 109.36 (12) |
C(3)—C(13)—H(13A) | 109.69 (15) | C(8)—C(18)—H(18A) | 109.90 (16) |
C(3)—C(13)—H(13B) | 109.36 (13) | C(8)—C(18)—H(18B) | 109.25 (14) |
C(3)—C(13)—H(13C) | 109.45 (14) | C(8)—C(18)—H(18C) | 109.60 (15) |
H(13A)—C(13)—H(13B) | 109.58 (15) | H(18A)—C(18)—H(18B) | 109.42 (17) |
H(13A)—C(13)—H(13C) | 109.58 (14) | H(18A)—C(18)—H(18C) | 109.70 (15) |
H(13B)—C(13)—H(13C) | 109.16 (17) | H(18B)—C(18)—H(18C) | 108.96 (17) |
C(4)—C(14)—H(14A) | 109.52 (17) | C(9)—C(19)—H(19A) | 109.58 (18) |
C(4)—C(14)—H(14B) | 109.60 (16) | C(9)—C(19)—H(19B) | 109.5 (2) |
C(4)—C(14)—H(14C) | 109.37 (16) | C(9)—C(19)—H(19C) | 109.70 (16) |
C(4)—C(14)—H(14D) | 109.47 (17) | C(9)—C(19)—H(19D) | 109.6 (2) |
C(4)—C(14)—H(14E) | 109.40 (17) | C(9)—C(19)—H(19E) | 109.68 (16) |
C(4)—C(14)—H(14F) | 109.62 (15) | C(9)—C(19)—H(19F) | 109.51 (19) |
H(14A)—C(14)—H(14B) | 109.65 (17) | H(19A)—C(19)—H(19B) | 109.19 (17) |
H(14A)—C(14)—H(14C) | 109.33 (17) | H(19A)—C(19)—H(19C) | 109.4 (2) |
H(14A)—C(14)—H(14D) | 141.0 (3) | H(19A)—C(19)—H(19D) | 140.8 (3) |
H(14A)—C(14)—H(14E) | 56.23 (10) | H(19A)—C(19)—H(19E) | 56.21 (12) |
H(14A)—C(14)—H(14F) | 56.36 (9) | H(19A)—C(19)—H(19F) | 56.12 (10) |
H(14B)—C(14)—H(14C) | 109.35 (18) | H(19B)—C(19)—H(19C) | 109.40 (19) |
H(14B)—C(14)—H(14D) | 56.25 (10) | H(19B)—C(19)—H(19D) | 56.19 (10) |
H(14B)—C(14)—H(14E) | 141.0 (3) | H(19B)—C(19)—H(19E) | 140.8 (3) |
H(14B)—C(14)—H(14F) | 56.36 (8) | H(19B)—C(19)—H(19F) | 56.11 (8) |
H(14C)—C(14)—H(14D) | 56.13 (9) | H(19C)—C(19)—H(19D) | 56.28 (10) |
H(14C)—C(14)—H(14E) | 56.12 (8) | H(19C)—C(19)—H(19E) | 56.29 (10) |
H(14C)—C(14)—H(14F) | 141.0 (3) | H(19C)—C(19)—H(19F) | 140.8 (3) |
H(14D)—C(14)—H(14E) | 109.24 (15) | H(19D)—C(19)—H(19E) | 109.5 (2) |
H(14D)—C(14)—H(14F) | 109.56 (18) | H(19D)—C(19)—H(19F) | 109.25 (16) |
H(14E)—C(14)—H(14F) | 109.54 (19) | H(19E)—C(19)—H(19F) | 109.3 (2) |
C(5)—C(15)—H(15A) | 109.49 (14) | C(10)—C(20)—H(20A) | 109.85 (14) |
C(5)—C(15)—H(15B) | 109.54 (11) | C(10)—C(20)—H(20B) | 109.57 (11) |
C(5)—C(15)—H(15C) | 109.68 (12) | C(10)—C(20)—H(20C) | 109.29 (12) |
C(5)—C(15)—H(15D) | 109.65 (15) | H(20A)—C(20)—H(20B) | 109.66 (13) |
C(5)—C(15)—H(15E) | 109.60 (11) | H(20A)—C(20)—H(20C) | 109.29 (11) |
C(5)—C(15)—H(15F) | 109.46 (9) | H(20B)—C(20)—H(20C) | 109.16 (15) |
C20H30Zn2 | V = 951.09 (8) Å3 |
Mr = 401.18 | Z = 2 |
Triclinic, P1 | F(000) = 64 |
a = 6.9329 (3) Å | Dx = 1.452 Mg m−3 |
b = 10.8831 (5) Å | White-beam radiation, λ = ? Å |
c = 13.8384 (7) Å | µ = 0.00 mm−1 |
α = 109.777 (1)° | T = 170 K |
β = 101.603 (1)° | Prismatic, colorless |
γ = 94.201 (1)° | 2.0 × 1.0 × 0.3 mm |
VIVALDI diffractometer | Rint = 0.364 |
Radiation source: nuclear reactor | θmax = 21.8°, θmin = 2.1° |
Laue scans | h = −7→7 |
8553 measured reflections | k = −11→11 |
1665 independent reflections | l = −14→14 |
985 reflections with I > 2σ(I) |
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)] = 0.105 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.264 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.1322P)2] where P = (Fo2 + 2Fc2)/3 |
1665 reflections | (Δ/σ)max = 0.032 |
469 parameters | Δρmax = 0.67 e Å−3 |
0 restraints | Δρmin = −0.60 e Å−3 |
C20H30Zn2 | γ = 94.201 (1)° |
Mr = 401.18 | V = 951.09 (8) Å3 |
Triclinic, P1 | Z = 2 |
a = 6.9329 (3) Å | White-beam radiation, λ = ? Å |
b = 10.8831 (5) Å | µ = 0.00 mm−1 |
c = 13.8384 (7) Å | T = 170 K |
α = 109.777 (1)° | 2.0 × 1.0 × 0.3 mm |
β = 101.603 (1)° |
VIVALDI diffractometer | 985 reflections with I > 2σ(I) |
8553 measured reflections | Rint = 0.364 |
1665 independent reflections |
R[F2 > 2σ(F2)] = 0.105 | 0 restraints |
wR(F2) = 0.264 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | Δρmax = 0.67 e Å−3 |
1665 reflections | Δρmin = −0.60 e Å−3 |
469 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 | ||
Zn1 | 0.3354 (13) | 0.2188 (6) | 0.3170 (6) | 0.032 (2) | |
Zn2 | 0.1478 (12) | 0.2910 (7) | 0.1964 (6) | 0.034 (2) | |
C1 | 0.6444 (11) | 0.2452 (7) | 0.4275 (5) | 0.034 (2) | |
C2 | 0.5964 (11) | 0.1082 (6) | 0.3514 (5) | 0.036 (2) | |
C3 | 0.4226 (12) | 0.0487 (6) | 0.3681 (6) | 0.043 (2) | |
C4 | 0.3618 (10) | 0.1462 (6) | 0.4541 (5) | 0.033 (2) | |
C5 | 0.5034 (12) | 0.2644 (7) | 0.4879 (6) | 0.042 (2) | |
C6 | −0.1044 (10) | 0.2337 (6) | 0.0429 (5) | 0.035 (2) | |
C7 | 0.0774 (12) | 0.2924 (7) | 0.0265 (6) | 0.045 (2) | |
C8 | 0.1200 (11) | 0.4255 (5) | 0.0980 (5) | 0.033 (2) | |
C9 | −0.0276 (12) | 0.4491 (6) | 0.1615 (5) | 0.038 (2) | |
C10 | −0.1627 (11) | 0.3272 (7) | 0.1241 (6) | 0.038 (2) | |
C11 | 0.8247 (16) | 0.3382 (10) | 0.4441 (10) | 0.045 (3) | |
H11A | 0.949 (6) | 0.331 (3) | 0.491 (3) | 0.146 (16) | |
H11B | 0.786 (4) | 0.438 (2) | 0.457 (3) | 0.160 (16) | |
H11C | 0.888 (4) | 0.319 (3) | 0.379 (2) | 0.135 (13) | |
C12 | 0.717 (2) | 0.0411 (12) | 0.2777 (8) | 0.049 (4) | |
H12A | 0.818 (4) | 0.106 (2) | 0.268 (2) | 0.118 (10) | |
H12B | 0.618 (3) | −0.002 (3) | 0.192 (2) | 0.139 (12) | |
H12C | 0.787 (6) | −0.015 (3) | 0.297 (3) | 0.109 (13) | |
C13 | 0.333 (2) | −0.0917 (8) | 0.3149 (11) | 0.058 (4) | |
H13A | 0.366 (5) | −0.144 (2) | 0.370 (2) | 0.123 (12) | |
H13B | 0.330 (7) | −0.134 (3) | 0.242 (3) | 0.19 (2) | |
H13C | 0.159 (4) | −0.1055 (18) | 0.301 (3) | 0.124 (11) | |
C14 | 0.202 (2) | 0.1151 (10) | 0.5041 (10) | 0.051 (3) | |
H14A | 0.237 (4) | 0.054 (4) | 0.541 (2) | 0.132 (13) | |
H14B | 0.061 (5) | 0.086 (3) | 0.458 (3) | 0.129 (13) | |
H14C | 0.189 (4) | 0.212 (2) | 0.572 (3) | 0.169 (15) | |
C15 | 0.501 (2) | 0.3856 (9) | 0.5771 (7) | 0.044 (3) | |
H15A | 0.364 (5) | 0.397 (3) | 0.593 (2) | 0.120 (11) | |
H15B | 0.569 (4) | 0.476 (2) | 0.5801 (18) | 0.115 (9) | |
H15C | 0.568 (5) | 0.378 (2) | 0.6570 (16) | 0.125 (12) | |
C16 | −0.213 (3) | 0.0954 (11) | −0.0242 (10) | 0.070 (5) | |
H16A | −0.266 (4) | 0.047 (2) | 0.0271 (18) | 0.104 (8) | |
H16B | −0.126 (4) | 0.037 (3) | −0.058 (3) | 0.134 (13) | |
H16C | −0.339 (4) | 0.099 (2) | −0.080 (2) | 0.103 (11) | |
C17 | 0.181 (2) | 0.2335 (12) | −0.0580 (9) | 0.052 (3) | |
H17A | 0.105 (4) | 0.223 (2) | −0.1349 (19) | 0.108 (9) | |
H17B | 0.197 (7) | 0.142 (3) | −0.065 (3) | 0.19 (2) | |
H17C | 0.312 (5) | 0.287 (4) | −0.0476 (17) | 0.114 (9) | |
C18 | 0.280 (2) | 0.5291 (11) | 0.0982 (8) | 0.048 (4) | |
H18A | 0.384 (4) | 0.493 (3) | 0.071 (4) | 0.133 (14) | |
H18B | 0.340 (4) | 0.6090 (19) | 0.1818 (16) | 0.099 (8) | |
H18C | 0.226 (4) | 0.578 (3) | 0.047 (3) | 0.120 (11) | |
C19 | −0.0499 (18) | 0.5739 (10) | 0.2397 (12) | 0.060 (4) | |
H19A | −0.176 (7) | 0.619 (3) | 0.211 (2) | 0.151 (15) | |
H19B | 0.088 (5) | 0.6464 (18) | 0.271 (3) | 0.161 (16) | |
H19C | −0.073 (5) | 0.560 (2) | 0.3091 (17) | 0.113 (9) | |
C20 | −0.3466 (19) | 0.3104 (10) | 0.1625 (10) | 0.048 (3) | |
H20A | −0.470 (4) | 0.326 (4) | 0.116 (3) | 0.125 (13) | |
H20B | −0.328 (4) | 0.363 (3) | 0.242 (2) | 0.145 (14) | |
H20C | −0.388 (4) | 0.217 (2) | 0.167 (3) | 0.159 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.047 (6) | 0.030 (4) | 0.023 (4) | −0.003 (4) | 0.008 (4) | 0.016 (3) |
Zn2 | 0.035 (6) | 0.041 (4) | 0.030 (5) | −0.001 (4) | 0.001 (4) | 0.023 (4) |
C1 | 0.033 (5) | 0.053 (4) | 0.028 (4) | 0.005 (4) | 0.000 (4) | 0.034 (3) |
C2 | 0.040 (5) | 0.033 (4) | 0.028 (4) | −0.003 (3) | −0.008 (4) | 0.012 (3) |
C3 | 0.046 (6) | 0.038 (4) | 0.039 (5) | −0.018 (4) | −0.017 (4) | 0.026 (4) |
C4 | 0.035 (5) | 0.043 (4) | 0.035 (4) | −0.003 (3) | 0.003 (4) | 0.036 (3) |
C5 | 0.047 (6) | 0.052 (4) | 0.032 (4) | −0.001 (4) | −0.002 (4) | 0.030 (4) |
C6 | 0.032 (5) | 0.051 (4) | 0.020 (4) | −0.007 (3) | −0.008 (4) | 0.023 (3) |
C7 | 0.043 (5) | 0.062 (5) | 0.034 (5) | −0.002 (4) | −0.001 (4) | 0.030 (4) |
C8 | 0.048 (5) | 0.033 (4) | 0.013 (4) | −0.012 (3) | −0.002 (4) | 0.010 (3) |
C9 | 0.057 (6) | 0.038 (4) | 0.023 (4) | 0.005 (4) | 0.015 (4) | 0.013 (3) |
C10 | 0.039 (5) | 0.047 (4) | 0.037 (4) | 0.002 (4) | 0.010 (4) | 0.030 (3) |
C11 | 0.040 (7) | 0.040 (5) | 0.057 (7) | −0.017 (6) | −0.011 (6) | 0.036 (5) |
H11A | 0.12 (3) | 0.13 (2) | 0.20 (4) | −0.06 (2) | −0.04 (3) | 0.13 (3) |
H11B | 0.10 (2) | 0.041 (12) | 0.32 (5) | −0.013 (12) | 0.07 (3) | 0.039 (17) |
H11C | 0.12 (2) | 0.18 (2) | 0.075 (14) | −0.089 (18) | 0.024 (17) | 0.037 (15) |
C12 | 0.072 (9) | 0.074 (8) | 0.008 (6) | 0.026 (7) | 0.012 (7) | 0.020 (5) |
H12A | 0.13 (2) | 0.083 (14) | 0.14 (2) | 0.012 (14) | 0.07 (2) | 0.014 (14) |
H12B | 0.065 (15) | 0.22 (3) | 0.057 (16) | 0.037 (16) | −0.018 (13) | −0.032 (17) |
H12C | 0.15 (3) | 0.14 (3) | 0.09 (2) | 0.08 (2) | 0.04 (2) | 0.084 (18) |
C13 | 0.060 (8) | 0.027 (5) | 0.068 (8) | −0.013 (5) | −0.004 (7) | 0.009 (6) |
H13A | 0.14 (3) | 0.077 (13) | 0.12 (2) | 0.000 (14) | −0.100 (19) | 0.076 (15) |
H13B | 0.34 (6) | 0.09 (2) | 0.11 (3) | −0.10 (3) | −0.02 (3) | 0.065 (19) |
H13C | 0.10 (2) | 0.064 (12) | 0.18 (3) | −0.051 (13) | 0.026 (19) | 0.026 (14) |
C14 | 0.046 (8) | 0.071 (6) | 0.059 (7) | 0.019 (6) | 0.014 (7) | 0.050 (6) |
H14A | 0.08 (2) | 0.27 (4) | 0.17 (3) | 0.07 (2) | 0.07 (2) | 0.18 (3) |
H14B | 0.071 (18) | 0.16 (2) | 0.15 (3) | −0.042 (19) | 0.018 (18) | 0.07 (2) |
H14C | 0.17 (3) | 0.092 (14) | 0.23 (3) | 0.004 (16) | 0.16 (3) | −0.029 (18) |
C15 | 0.065 (8) | 0.041 (5) | 0.017 (6) | 0.019 (5) | −0.012 (6) | 0.008 (4) |
H15A | 0.11 (2) | 0.14 (2) | 0.062 (18) | −0.017 (18) | 0.008 (18) | −0.006 (14) |
H15B | 0.20 (3) | 0.073 (13) | 0.095 (17) | 0.030 (15) | 0.085 (17) | 0.021 (12) |
H15C | 0.26 (4) | 0.104 (14) | 0.000 (11) | 0.101 (18) | −0.032 (14) | 0.024 (9) |
C16 | 0.106 (13) | 0.037 (6) | 0.054 (8) | −0.023 (8) | 0.004 (9) | 0.014 (6) |
H16A | 0.15 (2) | 0.073 (11) | 0.105 (16) | −0.016 (12) | 0.028 (17) | 0.061 (12) |
H16B | 0.10 (2) | 0.076 (15) | 0.17 (3) | −0.011 (14) | −0.01 (2) | −0.010 (17) |
H16C | 0.080 (19) | 0.081 (15) | 0.090 (19) | −0.034 (14) | −0.063 (15) | 0.013 (14) |
C17 | 0.061 (8) | 0.080 (8) | 0.019 (7) | 0.022 (6) | −0.004 (6) | 0.027 (5) |
H17A | 0.14 (2) | 0.17 (2) | 0.012 (11) | 0.043 (18) | 0.012 (14) | 0.035 (12) |
H17B | 0.38 (6) | 0.077 (15) | 0.20 (4) | 0.10 (2) | 0.23 (4) | 0.042 (18) |
H17C | 0.09 (2) | 0.18 (3) | 0.053 (14) | 0.05 (2) | 0.030 (15) | 0.007 (15) |
C18 | 0.066 (10) | 0.055 (6) | 0.021 (5) | −0.020 (6) | −0.006 (6) | 0.029 (5) |
H18A | 0.054 (19) | 0.107 (19) | 0.28 (4) | −0.010 (14) | 0.00 (2) | 0.14 (3) |
H18B | 0.15 (2) | 0.069 (11) | 0.052 (12) | −0.043 (12) | 0.013 (13) | 0.005 (10) |
H18C | 0.08 (2) | 0.12 (2) | 0.17 (3) | −0.020 (16) | −0.040 (19) | 0.11 (2) |
C19 | 0.058 (8) | 0.056 (6) | 0.082 (10) | 0.038 (6) | 0.028 (8) | 0.031 (6) |
H19A | 0.23 (4) | 0.092 (17) | 0.10 (2) | −0.03 (2) | −0.08 (2) | 0.071 (16) |
H19B | 0.19 (3) | 0.026 (8) | 0.27 (4) | 0.006 (14) | 0.15 (3) | 0.004 (13) |
H19C | 0.19 (3) | 0.121 (17) | 0.045 (13) | 0.063 (17) | 0.044 (17) | 0.032 (12) |
C20 | 0.054 (9) | 0.069 (6) | 0.047 (8) | 0.017 (6) | 0.018 (7) | 0.048 (5) |
H20A | 0.051 (19) | 0.22 (3) | 0.14 (3) | 0.04 (2) | 0.037 (19) | 0.09 (2) |
H20B | 0.12 (2) | 0.21 (3) | 0.046 (14) | −0.043 (18) | 0.020 (14) | −0.024 (16) |
H20C | 0.11 (2) | 0.107 (17) | 0.35 (5) | 0.036 (16) | 0.13 (3) | 0.16 (3) |
Zn1—Zn2 | 2.292 (14) | C12—H12C | 0.89 (4) |
C1—C5 | 1.392 (10) | C13—H13A | 1.09 (4) |
C1—C2 | 1.472 (9) | C13—H13B | 0.95 (5) |
C1—C11 | 1.477 (11) | C13—H13C | 1.17 (4) |
C2—C3 | 1.423 (10) | C14—H14A | 0.98 (4) |
C2—C12 | 1.485 (11) | C14—H14B | 1.02 (5) |
C3—C4 | 1.460 (10) | C14—H14C | 1.17 (2) |
C3—C13 | 1.476 (11) | C15—H15A | 1.03 (4) |
C4—C5 | 1.436 (9) | C15—H15B | 1.05 (3) |
C4—C14 | 1.492 (11) | C15—H15C | 1.15 (3) |
C5—C15 | 1.474 (11) | C16—H16A | 1.12 (2) |
C6—C10 | 1.390 (10) | C16—H16B | 0.98 (5) |
C6—C7 | 1.464 (9) | C16—H16C | 1.06 (5) |
C6—C16 | 1.516 (12) | C17—H17A | 1.05 (4) |
C7—C8 | 1.420 (9) | C17—H17B | 0.98 (4) |
C7—C17 | 1.482 (13) | C17—H17C | 0.99 (5) |
C8—C9 | 1.460 (9) | C18—H18A | 0.93 (5) |
C8—C18 | 1.520 (10) | C18—H18B | 1.16 (2) |
C9—C10 | 1.437 (10) | C18—H18C | 1.04 (4) |
C9—C19 | 1.464 (12) | C19—H19A | 1.11 (5) |
C10—C20 | 1.498 (12) | C19—H19B | 1.10 (4) |
C11—H11A | 0.99 (5) | C19—H19C | 1.06 (3) |
C11—H11B | 1.11 (3) | C20—H20A | 1.02 (5) |
C11—H11C | 1.04 (3) | C20—H20B | 1.03 (3) |
C12—H12A | 1.02 (4) | C20—H20C | 1.06 (2) |
C12—H12B | 1.16 (3) | ||
C5—C1—C2 | 107.7 (6) | C3—C13—H13C | 111.7 (13) |
C5—C1—C11 | 126.8 (7) | H13A—C13—H13C | 99 (2) |
C2—C1—C11 | 125.1 (7) | H13B—C13—H13C | 94 (3) |
C3—C2—C1 | 107.3 (6) | C4—C14—H14A | 112.3 (15) |
C3—C2—C12 | 126.3 (7) | C4—C14—H14B | 117.0 (17) |
C1—C2—C12 | 126.3 (7) | H14A—C14—H14B | 111 (3) |
C2—C3—C4 | 108.4 (5) | C4—C14—H14C | 108.5 (13) |
C2—C3—C13 | 125.3 (8) | H14A—C14—H14C | 104 (3) |
C4—C3—C13 | 126.0 (7) | H14B—C14—H14C | 103 (2) |
C5—C4—C3 | 106.4 (5) | C5—C15—H15A | 114.6 (14) |
C5—C4—C14 | 129.0 (7) | C5—C15—H15B | 119.1 (13) |
C3—C4—C14 | 124.0 (6) | H15A—C15—H15B | 109 (2) |
C1—C5—C4 | 110.3 (6) | C5—C15—H15C | 111.8 (12) |
C1—C5—C15 | 125.9 (8) | H15A—C15—H15C | 93 (2) |
C4—C5—C15 | 123.8 (7) | H15B—C15—H15C | 106 (2) |
C10—C6—C7 | 108.9 (6) | C6—C16—H16A | 109.9 (14) |
C10—C6—C16 | 127.2 (8) | C6—C16—H16B | 112.9 (17) |
C7—C6—C16 | 123.9 (8) | H16A—C16—H16B | 104 (3) |
C8—C7—C6 | 106.4 (6) | C6—C16—H16C | 110.6 (17) |
C8—C7—C17 | 125.5 (7) | H16A—C16—H16C | 108 (2) |
C6—C7—C17 | 127.6 (7) | H16B—C16—H16C | 112 (3) |
C7—C8—C9 | 109.1 (5) | C7—C17—H17A | 115.3 (17) |
C7—C8—C18 | 124.5 (6) | C7—C17—H17B | 110.3 (16) |
C9—C8—C18 | 126.1 (6) | H17A—C17—H17B | 103 (3) |
C10—C9—C8 | 106.0 (5) | C7—C17—H17C | 113.0 (15) |
C10—C9—C19 | 125.7 (7) | H17A—C17—H17C | 104 (2) |
C8—C9—C19 | 128.0 (7) | H17B—C17—H17C | 111 (3) |
C6—C10—C9 | 109.6 (5) | C8—C18—H18A | 113.4 (15) |
C6—C10—C20 | 126.3 (7) | C8—C18—H18B | 111.5 (10) |
C9—C10—C20 | 123.9 (7) | H18A—C18—H18B | 111 (2) |
C1—C11—H11A | 117.1 (13) | C8—C18—H18C | 112.1 (15) |
C1—C11—H11B | 109.6 (14) | H18A—C18—H18C | 101 (3) |
H11A—C11—H11B | 118 (3) | H18B—C18—H18C | 107 (2) |
C1—C11—H11C | 114.8 (14) | C9—C19—H19A | 113.4 (18) |
H11A—C11—H11C | 93 (3) | C9—C19—H19B | 112.9 (13) |
H11B—C11—H11C | 103 (3) | H19A—C19—H19B | 110 (2) |
C2—C12—H12A | 112.5 (14) | C9—C19—H19C | 110.8 (16) |
C2—C12—H12B | 109.1 (14) | H19A—C19—H19C | 107 (3) |
H12A—C12—H12B | 99 (2) | H19B—C19—H19C | 102 (3) |
C2—C12—H12C | 114.9 (18) | C10—C20—H20A | 112.6 (16) |
H12A—C12—H12C | 106 (3) | C10—C20—H20B | 113.0 (16) |
H12B—C12—H12C | 115 (3) | H20A—C20—H20B | 113 (3) |
C3—C13—H13A | 109.8 (15) | C10—C20—H20C | 116.8 (15) |
C3—C13—H13B | 118.6 (14) | H20A—C20—H20C | 105 (2) |
H13A—C13—H13B | 121 (2) | H20B—C20—H20C | 95 (3) |
Experimental details
(znzn) | (zn-zn) | |
Crystal data | ||
Chemical formula | C20H30Zn2 | C20H30Zn2 |
Mr | 401.18 | 401.18 |
Crystal system, space group | Triclinic, P1 | Triclinic, P1 |
Temperature (K) | 100 | 170 |
a, b, c (Å) | 6.9115 (6), 10.8895 (14), 13.8927 (14) | 6.9329 (3), 10.8831 (5), 13.8384 (7) |
α, β, γ (°) | 109.908 (10), 101.551 (8), 93.905 (9) | 109.777 (1), 101.603 (1), 94.201 (1) |
V (Å3) | 952.61 (18) | 951.09 (8) |
Z | 2 | 2 |
Radiation type | Synchrotron, λ = 0.71000 Å | White-beam, λ = ? Å |
µ (mm−1) | 2.51 | 0.00 |
Crystal size (mm) | 0.70 × 0.70 × 0.05 | 2.0 × 1.0 × 0.3 |
Data collection | ||
Diffractometer | CCD area detector diffractometer | VIVALDI diffractometer |
Absorption correction | Multi-scan SADABS | – |
Tmin, Tmax | 0.272, 0.881 | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 57003, 13873, 12354 | 8553, 1665, 985 |
Rint | 0.054 | 0.364 |
(sin θ/λ)max (Å−1) | 0.970 | – |
Distance from specimen to detector (mm) | – | h = −7→7, k = −11→11, l = −14→14 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.036, 0.040, 1.10 | 0.105, 0.264, 1.08 |
No. of reflections | 11249 | 1665 |
No. of parameters | 782 | 469 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.59, −0.48 | 0.67, −0.60 |
Computer programs: CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05), LAUEGEN, CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05)
SORTAV (Blessing, 1989), ARGONNE BOXES, SHELXS97 (Sheldrick, 1997), XD2006 (Volkov et al., 2006), SHELXL97 (Sheldrick, 1997), SHELXTL.
ZN(1)—ZN(2) | 2.3186 (3) | C(14)—H(14C) | 1.0495 (14) |
C(1)—C(2) | 1.4358 (15) | C(14)—H(14D) | 1.0495 (19) |
C(1)—C(5) | 1.436 (2) | C(14)—H(14E) | 1.0495 (17) |
C(1)—C(11) | 1.502 (3) | C(14)—H(14F) | 1.0495 (15) |
C(2)—C(3) | 1.430 (3) | C(15)—H(15A) | 1.050 (2) |
C(2)—C(12) | 1.504 (2) | C(15)—H(15B) | 1.0495 (14) |
C(3)—C(4) | 1.444 (2) | C(15)—H(15C) | 1.0495 (12) |
C(3)—C(13) | 1.5051 (17) | C(15)—H(15D) | 1.0495 (19) |
C(4)—C(5) | 1.438 (2) | C(15)—H(15E) | 1.0495 (14) |
C(4)—C(14) | 1.496 (3) | C(15)—H(15F) | 1.0495 (14) |
C(5)—C(15) | 1.5066 (14) | C(16)—H(16A) | 1.049 (2) |
C(6)—C(7) | 1.4357 (16) | C(16)—H(16B) | 1.0495 (14) |
C(6)—C(10) | 1.438 (2) | C(16)—H(16C) | 1.0495 (15) |
C(6)—C(16) | 1.505 (3) | C(16)—H(16D) | 1.0495 (17) |
C(7)—C(8) | 1.431 (3) | C(16)—H(16E) | 1.0495 (17) |
C(7)—C(17) | 1.502 (2) | C(16)—H(16F) | 1.049 (2) |
C(8)—C(9) | 1.441 (2) | C(17)—H(17A) | 1.049 (2) |
C(8)—C(18) | 1.5022 (19) | C(17)—H(17B) | 1.0495 (11) |
C(9)—C(10) | 1.439 (2) | C(17)—H(17C) | 1.0495 (13) |
C(9)—C(19) | 1.492 (3) | C(18)—H(18A) | 1.050 (3) |
C(10)—C(20) | 1.5067 (16) | C(18)—H(18B) | 1.0495 (17) |
C(11)—H(11A) | 1.050 (2) | C(18)—H(18C) | 1.0495 (15) |
C(11)—H(11B) | 1.0495 (12) | C(19)—H(19A) | 1.049 (2) |
C(11)—H(11C) | 1.0495 (14) | C(19)—H(19B) | 1.0495 (17) |
C(12)—H(12A) | 1.050 (2) | C(19)—H(19C) | 1.0495 (19) |
C(12)—H(12B) | 1.0495 (12) | C(19)—H(19D) | 1.050 (2) |
C(12)—H(12C) | 1.0495 (13) | C(19)—H(19E) | 1.050 (2) |
C(13)—H(13A) | 1.049 (3) | C(19)—H(19F) | 1.0495 (16) |
C(13)—H(13B) | 1.0495 (15) | C(20)—H(20A) | 1.050 (2) |
C(13)—H(13C) | 1.0495 (14) | C(20)—H(20B) | 1.0495 (13) |
C(14)—H(14A) | 1.0495 (19) | C(20)—H(20C) | 1.0495 (14) |
C(14)—H(14B) | 1.0495 (18) | ||
C(2)—C(1)—C(5) | 108.04 (15) | H(15A)—C(15)—H(15B) | 109.19 (13) |
C(2)—C(1)—C(11) | 125.91 (17) | H(15A)—C(15)—H(15C) | 109.43 (11) |
C(5)—C(1)—C(11) | 125.83 (11) | H(15A)—C(15)—H(15D) | 140.86 (11) |
C(1)—C(2)—C(3) | 107.82 (14) | H(15A)—C(15)—H(15E) | 56.19 (9) |
C(1)—C(2)—C(12) | 126.44 (18) | H(15A)—C(15)—H(15F) | 56.10 (10) |
C(3)—C(2)—C(12) | 125.31 (13) | H(15B)—C(15)—H(15C) | 109.49 (15) |
C(2)—C(3)—C(4) | 108.63 (11) | H(15B)—C(15)—H(15D) | 56.24 (9) |
C(2)—C(3)—C(13) | 125.01 (15) | H(15B)—C(15)—H(15E) | 140.85 (11) |
C(4)—C(3)—C(13) | 126.07 (19) | H(15B)—C(15)—H(15F) | 56.12 (6) |
C(3)—C(4)—C(5) | 107.11 (16) | H(15C)—C(15)—H(15D) | 56.32 (9) |
C(3)—C(4)—C(14) | 125.91 (14) | H(15C)—C(15)—H(15E) | 56.30 (5) |
C(5)—C(4)—C(14) | 126.84 (13) | H(15C)—C(15)—H(15F) | 140.85 (11) |
C(1)—C(5)—C(4) | 108.39 (11) | H(15D)—C(15)—H(15E) | 109.55 (10) |
C(1)—C(5)—C(15) | 125.27 (15) | H(15D)—C(15)—H(15F) | 109.31 (12) |
C(4)—C(5)—C(15) | 126.16 (17) | H(15E)—C(15)—H(15F) | 109.25 (17) |
C(7)—C(6)—C(10) | 108.12 (16) | C(6)—C(16)—H(16A) | 109.47 (14) |
C(7)—C(6)—C(16) | 124.80 (17) | C(6)—C(16)—H(16B) | 109.40 (16) |
C(10)—C(6)—C(16) | 126.96 (12) | C(6)—C(16)—H(16C) | 109.41 (19) |
C(6)—C(7)—C(8) | 107.96 (14) | C(6)—C(16)—H(16D) | 109.4 (2) |
C(6)—C(7)—C(17) | 125.56 (18) | C(6)—C(16)—H(16E) | 109.45 (14) |
C(8)—C(7)—C(17) | 126.25 (13) | C(6)—C(16)—H(16F) | 109.44 (13) |
C(7)—C(8)—C(9) | 108.32 (12) | H(16A)—C(16)—H(16B) | 109.5 (2) |
C(7)—C(8)—C(18) | 125.23 (16) | H(16A)—C(16)—H(16C) | 109.73 (17) |
C(9)—C(8)—C(18) | 126.1 (2) | H(16A)—C(16)—H(16D) | 141.1 (2) |
C(8)—C(9)—C(10) | 107.62 (17) | H(16A)—C(16)—H(16E) | 56.41 (11) |
C(8)—C(9)—C(19) | 125.58 (16) | H(16A)—C(16)—H(16F) | 56.32 (12) |
C(10)—C(9)—C(19) | 126.56 (14) | H(16B)—C(16)—H(16C) | 109.34 (14) |
C(6)—C(10)—C(9) | 107.98 (11) | H(16B)—C(16)—H(16D) | 56.12 (8) |
C(6)—C(10)—C(20) | 125.98 (15) | H(16B)—C(16)—H(16E) | 141.1 (2) |
C(9)—C(10)—C(20) | 125.63 (17) | H(16B)—C(16)—H(16F) | 56.17 (9) |
C(1)—C(11)—H(11A) | 109.64 (12) | H(16C)—C(16)—H(16D) | 56.21 (8) |
C(1)—C(11)—H(11B) | 109.43 (16) | H(16C)—C(16)—H(16E) | 56.36 (8) |
C(1)—C(11)—H(11C) | 109.40 (15) | H(16C)—C(16)—H(16F) | 141.1 (2) |
H(11A)—C(11)—H(11B) | 109.63 (17) | H(16D)—C(16)—H(16E) | 109.55 (14) |
H(11A)—C(11)—H(11C) | 109.53 (17) | H(16D)—C(16)—H(16F) | 109.31 (14) |
H(11B)—C(11)—H(11C) | 109.20 (13) | H(16E)—C(16)—H(16F) | 109.7 (2) |
C(2)—C(12)—H(12A) | 109.51 (12) | C(7)—C(17)—H(17A) | 109.49 (12) |
C(2)—C(12)—H(12B) | 109.39 (14) | C(7)—C(17)—H(17B) | 109.43 (15) |
C(2)—C(12)—H(12C) | 109.46 (15) | C(7)—C(17)—H(17C) | 109.42 (14) |
H(12A)—C(12)—H(12B) | 109.55 (16) | H(17A)—C(17)—H(17B) | 109.54 (15) |
H(12A)—C(12)—H(12C) | 109.62 (16) | H(17A)—C(17)—H(17C) | 109.58 (17) |
H(12B)—C(12)—H(12C) | 109.30 (13) | H(17B)—C(17)—H(17C) | 109.36 (12) |
C(3)—C(13)—H(13A) | 109.69 (15) | C(8)—C(18)—H(18A) | 109.90 (16) |
C(3)—C(13)—H(13B) | 109.36 (13) | C(8)—C(18)—H(18B) | 109.25 (14) |
C(3)—C(13)—H(13C) | 109.45 (14) | C(8)—C(18)—H(18C) | 109.60 (15) |
H(13A)—C(13)—H(13B) | 109.58 (15) | H(18A)—C(18)—H(18B) | 109.42 (17) |
H(13A)—C(13)—H(13C) | 109.58 (14) | H(18A)—C(18)—H(18C) | 109.70 (15) |
H(13B)—C(13)—H(13C) | 109.16 (17) | H(18B)—C(18)—H(18C) | 108.96 (17) |
C(4)—C(14)—H(14A) | 109.52 (17) | C(9)—C(19)—H(19A) | 109.58 (18) |
C(4)—C(14)—H(14B) | 109.60 (16) | C(9)—C(19)—H(19B) | 109.5 (2) |
C(4)—C(14)—H(14C) | 109.37 (16) | C(9)—C(19)—H(19C) | 109.70 (16) |
C(4)—C(14)—H(14D) | 109.47 (17) | C(9)—C(19)—H(19D) | 109.6 (2) |
C(4)—C(14)—H(14E) | 109.40 (17) | C(9)—C(19)—H(19E) | 109.68 (16) |
C(4)—C(14)—H(14F) | 109.62 (15) | C(9)—C(19)—H(19F) | 109.51 (19) |
H(14A)—C(14)—H(14B) | 109.65 (17) | H(19A)—C(19)—H(19B) | 109.19 (17) |
H(14A)—C(14)—H(14C) | 109.33 (17) | H(19A)—C(19)—H(19C) | 109.4 (2) |
H(14A)—C(14)—H(14D) | 141.0 (3) | H(19A)—C(19)—H(19D) | 140.8 (3) |
H(14A)—C(14)—H(14E) | 56.23 (10) | H(19A)—C(19)—H(19E) | 56.21 (12) |
H(14A)—C(14)—H(14F) | 56.36 (9) | H(19A)—C(19)—H(19F) | 56.12 (10) |
H(14B)—C(14)—H(14C) | 109.35 (18) | H(19B)—C(19)—H(19C) | 109.40 (19) |
H(14B)—C(14)—H(14D) | 56.25 (10) | H(19B)—C(19)—H(19D) | 56.19 (10) |
H(14B)—C(14)—H(14E) | 141.0 (3) | H(19B)—C(19)—H(19E) | 140.8 (3) |
H(14B)—C(14)—H(14F) | 56.36 (8) | H(19B)—C(19)—H(19F) | 56.11 (8) |
H(14C)—C(14)—H(14D) | 56.13 (9) | H(19C)—C(19)—H(19D) | 56.28 (10) |
H(14C)—C(14)—H(14E) | 56.12 (8) | H(19C)—C(19)—H(19E) | 56.29 (10) |
H(14C)—C(14)—H(14F) | 141.0 (3) | H(19C)—C(19)—H(19F) | 140.8 (3) |
H(14D)—C(14)—H(14E) | 109.24 (15) | H(19D)—C(19)—H(19E) | 109.5 (2) |
H(14D)—C(14)—H(14F) | 109.56 (18) | H(19D)—C(19)—H(19F) | 109.25 (16) |
H(14E)—C(14)—H(14F) | 109.54 (19) | H(19E)—C(19)—H(19F) | 109.3 (2) |
C(5)—C(15)—H(15A) | 109.49 (14) | C(10)—C(20)—H(20A) | 109.85 (14) |
C(5)—C(15)—H(15B) | 109.54 (11) | C(10)—C(20)—H(20B) | 109.57 (11) |
C(5)—C(15)—H(15C) | 109.68 (12) | C(10)—C(20)—H(20C) | 109.29 (12) |
C(5)—C(15)—H(15D) | 109.65 (15) | H(20A)—C(20)—H(20B) | 109.66 (13) |
C(5)—C(15)—H(15E) | 109.60 (11) | H(20A)—C(20)—H(20C) | 109.29 (11) |
C(5)—C(15)—H(15F) | 109.46 (9) | H(20B)—C(20)—H(20C) | 109.16 (15) |
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