Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806052068/ci2220sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806052068/ci2220Isup2.hkl |
CCDC reference: 633644
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.024
- wR factor = 0.065
- Data-to-parameter ratio = 20.2
checkCIF/PLATON results
No syntax errors found
Alert level B REFLT03_ALERT_3_B Reflection count < 90% complete (theta max?) From the CIF: _diffrn_reflns_theta_max 26.99 From the CIF: _diffrn_reflns_theta_full 25.00 From the CIF: _reflns_number_total 1477 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 1656 Completeness (_total/calc) 89.19% PLAT022_ALERT_3_B Ratio Unique / Expected Reflections too Low .... 0.89 PLAT028_ALERT_3_B _diffrn_measured_fraction_theta_max Low ....... 0.89
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
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003); software used to prepare material for publication: SHELXL97.
[Zn(C3H7)2(C6H16N2)] | F(000) = 584 |
Mr = 267.75 | Dx = 1.175 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 5464 reflections |
a = 14.370 (4) Å | θ = 5.0–27.0° |
b = 8.5935 (16) Å | µ = 1.60 mm−1 |
c = 12.684 (3) Å | T = 293 K |
β = 104.928 (8)° | Needle, colourless |
V = 1513.4 (6) Å3 | 0.2 × 0.08 × 0.08 mm |
Z = 4 |
Rigaku R-AXIS IIC image-plate system diffractometer | 1477 independent reflections |
Radiation source: rotating-anode X-ray tube, Rigaku RU-H3R | 1407 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 105 pixels mm-1 | θmax = 27.0°, θmin = 5.0° |
φ scans | h = −18→17 |
Absorption correction: multi-scan (CrystalClear; Rigaku, 2000) | k = −10→10 |
Tmin = 0.724, Tmax = 0.883 | l = −16→15 |
5464 measured reflections |
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)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.065 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0453P)2 + 0.2577P] where P = (Fo2 + 2Fc2)/3 |
1477 reflections | (Δ/σ)max = 0.001 |
73 parameters | Δρmax = 0.71 e Å−3 |
0 restraints | Δρmin = −0.52 e Å−3 |
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 | 0.11058 (11) | 0.29879 (19) | 0.43429 (13) | 0.0226 (3) | |
H1A | 0.1637 | 0.2299 | 0.4370 | 0.034* | |
H1B | 0.1165 | 0.3431 | 0.5052 | 0.034* | |
H1C | 0.1108 | 0.3804 | 0.3827 | 0.034* | |
C2 | 0.01558 (10) | 0.20726 (16) | 0.39899 (10) | 0.0149 (3) | |
H2 | 0.0168 | 0.1242 | 0.4523 | 0.018* | |
C3 | −0.06841 (11) | 0.31554 (18) | 0.39951 (12) | 0.0210 (3) | |
H3A | −0.1272 | 0.2569 | 0.3835 | 0.031* | |
H3B | −0.0725 | 0.3950 | 0.3453 | 0.031* | |
H3C | −0.0583 | 0.3629 | 0.4701 | 0.031* | |
C4 | −0.04513 (11) | −0.22989 (17) | 0.27070 (13) | 0.0202 (3) | |
H4A | −0.0815 | −0.3242 | 0.2467 | 0.024* | |
H4B | −0.0269 | −0.2294 | 0.3498 | 0.024* | |
C5 | −0.15901 (12) | −0.11498 (17) | 0.11480 (13) | 0.0213 (3) | |
H5A | −0.1139 | −0.1179 | 0.0706 | 0.032* | |
H5B | −0.2031 | −0.0302 | 0.0918 | 0.032* | |
H5C | −0.1942 | −0.2111 | 0.1069 | 0.032* | |
C6 | −0.17632 (11) | −0.0722 (2) | 0.29621 (13) | 0.0217 (3) | |
H6A | −0.1425 | −0.0552 | 0.3711 | 0.033* | |
H6B | −0.2155 | −0.1638 | 0.2908 | 0.033* | |
H6C | −0.2165 | 0.0160 | 0.2696 | 0.033* | |
N1 | −0.10647 (9) | −0.09313 (13) | 0.23053 (10) | 0.0151 (3) | |
Zn1 | 0.0000 | 0.10820 (2) | 0.2500 | 0.01190 (11) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0196 (7) | 0.0262 (8) | 0.0209 (7) | −0.0057 (6) | 0.0030 (6) | −0.0067 (6) |
C2 | 0.0143 (6) | 0.0211 (7) | 0.0086 (6) | −0.0023 (5) | 0.0020 (5) | −0.0007 (5) |
C3 | 0.0217 (7) | 0.0226 (7) | 0.0189 (7) | 0.0049 (6) | 0.0055 (6) | −0.0002 (5) |
C4 | 0.0211 (8) | 0.0179 (7) | 0.0206 (7) | −0.0021 (5) | 0.0033 (6) | 0.0026 (5) |
C5 | 0.0182 (8) | 0.0300 (8) | 0.0129 (7) | −0.0074 (5) | −0.0007 (6) | −0.0021 (5) |
C6 | 0.0160 (7) | 0.0331 (8) | 0.0171 (7) | −0.0052 (6) | 0.0062 (6) | −0.0019 (6) |
N1 | 0.0121 (6) | 0.0208 (6) | 0.0113 (6) | −0.0023 (4) | 0.0010 (5) | −0.0001 (4) |
Zn1 | 0.01033 (15) | 0.01612 (15) | 0.00858 (14) | 0.000 | 0.00121 (9) | 0.000 |
C1—C2 | 1.5387 (19) | C4—H4B | 0.97 |
C1—H1A | 0.96 | C5—N1 | 1.4796 (19) |
C1—H1B | 0.96 | C5—H5A | 0.96 |
C1—H1C | 0.96 | C5—H5B | 0.96 |
C2—C3 | 1.525 (2) | C5—H5C | 0.96 |
C2—Zn1 | 2.0318 (14) | C6—N1 | 1.471 (2) |
C2—H2 | 0.98 | C6—H6A | 0.96 |
C3—H3A | 0.96 | C6—H6B | 0.96 |
C3—H3B | 0.96 | C6—H6C | 0.96 |
C3—H3C | 0.96 | N1—Zn1 | 2.2804 (13) |
C4—N1 | 1.4786 (19) | Zn1—C2i | 2.0318 (14) |
C4—C4i | 1.519 (3) | Zn1—N1i | 2.2804 (13) |
C4—H4A | 0.97 | ||
C2—C1—H1A | 109.5 | N1—C5—H5A | 109.5 |
C2—C1—H1B | 109.5 | N1—C5—H5B | 109.5 |
H1A—C1—H1B | 109.5 | H5A—C5—H5B | 109.5 |
C2—C1—H1C | 109.5 | N1—C5—H5C | 109.5 |
H1A—C1—H1C | 109.5 | H5A—C5—H5C | 109.5 |
H1B—C1—H1C | 109.5 | H5B—C5—H5C | 109.5 |
C3—C2—C1 | 109.30 (12) | N1—C6—H6A | 109.5 |
C3—C2—Zn1 | 111.22 (9) | N1—C6—H6B | 109.5 |
C1—C2—Zn1 | 111.21 (9) | H6A—C6—H6B | 109.5 |
C3—C2—H2 | 108.3 | N1—C6—H6C | 109.5 |
C1—C2—H2 | 108.3 | H6A—C6—H6C | 109.5 |
Zn1—C2—H2 | 108.3 | H6B—C6—H6C | 109.5 |
C2—C3—H3A | 109.5 | C6—N1—C4 | 109.58 (12) |
C2—C3—H3B | 109.5 | C6—N1—C5 | 109.21 (12) |
H3A—C3—H3B | 109.5 | C4—N1—C5 | 110.33 (12) |
C2—C3—H3C | 109.5 | C6—N1—Zn1 | 112.49 (9) |
H3A—C3—H3C | 109.5 | C4—N1—Zn1 | 104.00 (9) |
H3B—C3—H3C | 109.5 | C5—N1—Zn1 | 111.12 (9) |
N1—C4—C4i | 111.54 (11) | C2—Zn1—C2i | 130.46 (8) |
N1—C4—H4A | 109.3 | C2—Zn1—N1 | 109.19 (5) |
C4i—C4—H4A | 109.3 | C2i—Zn1—N1 | 107.88 (5) |
N1—C4—H4B | 109.3 | C2—Zn1—N1i | 107.88 (5) |
C4i—C4—H4B | 109.3 | C2i—Zn1—N1i | 109.19 (5) |
H4A—C4—H4B | 108.0 | N1—Zn1—N1i | 81.31 (7) |
Symmetry code: (i) −x, y, −z+1/2. |