Buy article online - an online subscription or single-article purchase is required to access this article.
The accuracy that can be achieved in single-pulse pump-probe Laue experiments is discussed. It is shown that with careful tuning of the experimental conditions a reproducibility of the intensity ratios of equivalent intensities obtained in different measurements of 3-4% can be achieved. The single-pulse experiments maximize the time resolution that can be achieved and, unlike stroboscopic techniques in which the pump-probe cycle is rapidly repeated, minimize the temperature increase due to the laser exposure of the sample.
Supporting information
CCDC reference: 767793
Crystals of title compound were obtained according to the literature (see for example Ford et al., 1999).
C—H hydrogen atoms were initially located in a difference Fourier map and were refined with a riding model. These atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with C—H distances in the range 0.95 − 1.00 Å. Uiso values were fixed such that they were 1.2Ueq of their parent atom Ueq for CH's and 1.5Ueq of their parent atom Ueq in case of methyl groups. The N—H hydrogen atoms was freely refined (Sheldrick, 2008).
Data collection: Data collection monitored with APEX2
APEX2 (ver. v2009.11-0), Bruker AXS (2009); cell refinement: Cell determination and refinement perfomed with APEX2
APEX2 (ver. v200911-0), Bruker AXS (2009); data reduction: Integration performed with SAINT
SAINT (ver. V7.68A), Bruker AXS (2009); program(s) used to solve structure: Solved with SHELXS97
Sheldrick, G. M.: (2008) Acta Cryst. A64, 112-122; program(s) used to refine structure: Refined with SHELXL97
Sheldrick, G. M.: (2008) Acta Cryst. A64, 112-122.
tetrakis((µ
3-iodo)-piperidine copper(I))
top
Crystal data top
C20H44Cu4I4N4 | Dx = 2.274 Mg m−3 |
Mr = 1102.39 | Melting point: not measured K |
Tetragonal, P42/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 4bc | Cell parameters from 7987 reflections |
a = 14.6049 (12) Å | θ = 2.8–30.3° |
c = 7.5464 (12) Å | µ = 6.46 mm−1 |
V = 1609.7 (3) Å3 | T = 90 K |
Z = 2 | Block, yellow |
F(000) = 1040 | 0.10 × 0.02 × 0.02 mm |
Data collection top
Bruker SMART APEXII CCD diffractometer | 2460 independent reflections |
Radiation source: Rigaku rotating anode | 2056 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.077 |
ω scans | θmax = 30.5°, θmin = 3.3° |
Absorption correction: multi-scan Absorption correction done by SORTAV
Blessing, R. H.: (1995) Acta Cryst. A51, 33-38 | h = −20→20 |
Tmin = 0.589, Tmax = 1.155 | k = −20→20 |
33915 measured reflections | l = −10→10 |
Refinement top
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) = 0.060 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0105P)2 + 1.0213P] where P = (Fo2 + 2Fc2)/3 |
2460 reflections | (Δ/σ)max = 0.002 |
77 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −1.51 e Å−3 |
Crystal data top
C20H44Cu4I4N4 | Z = 2 |
Mr = 1102.39 | Mo Kα radiation |
Tetragonal, P42/n | µ = 6.46 mm−1 |
a = 14.6049 (12) Å | T = 90 K |
c = 7.5464 (12) Å | 0.10 × 0.02 × 0.02 mm |
V = 1609.7 (3) Å3 | |
Data collection top
Bruker SMART APEXII CCD diffractometer | 2460 independent reflections |
Absorption correction: multi-scan Absorption correction done by SORTAV
Blessing, R. H.: (1995) Acta Cryst. A51, 33-38 | 2056 reflections with I > 2σ(I) |
Tmin = 0.589, Tmax = 1.155 | Rint = 0.077 |
33915 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.024 | 0 restraints |
wR(F2) = 0.060 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | Δρmax = 0.60 e Å−3 |
2460 reflections | Δρmin = −1.51 e Å−3 |
77 parameters | |
Special details top
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) top | x | y | z | Uiso*/Ueq | |
I1 | 0.773669 (11) | 0.594696 (11) | 0.04554 (2) | 0.01247 (6) | |
Cu1 | 0.66225 (2) | 0.73564 (2) | 0.12409 (4) | 0.01304 (8) | |
N1 | 0.55194 (15) | 0.72116 (15) | −0.0420 (3) | 0.0117 (4) | |
C1 | 0.48374 (19) | 0.79537 (19) | −0.0195 (4) | 0.0174 (5) | |
H1A | 0.5146 | 0.8551 | −0.0356 | 0.021* | |
H1B | 0.4595 | 0.7933 | 0.1030 | 0.021* | |
C3 | 0.35720 (18) | 0.69503 (19) | −0.1373 (4) | 0.0183 (5) | |
H3A | 0.3104 | 0.6897 | −0.2315 | 0.022* | |
H3B | 0.3261 | 0.6890 | −0.0213 | 0.022* | |
C2 | 0.40415 (18) | 0.78870 (19) | −0.1492 (4) | 0.0177 (5) | |
H2A | 0.4270 | 0.7983 | −0.2713 | 0.021* | |
H2B | 0.3591 | 0.8374 | −0.1228 | 0.021* | |
C5 | 0.50760 (18) | 0.62964 (19) | −0.0283 (4) | 0.0164 (5) | |
H5A | 0.4846 | 0.6209 | 0.0939 | 0.020* | |
H5B | 0.5539 | 0.5816 | −0.0518 | 0.020* | |
C4 | 0.42821 (18) | 0.61837 (19) | −0.1582 (4) | 0.0177 (5) | |
H4A | 0.3983 | 0.5585 | −0.1378 | 0.021* | |
H4B | 0.4522 | 0.6189 | −0.2809 | 0.021* | |
H1 | 0.576 (2) | 0.7281 (19) | −0.165 (4) | 0.005 (7)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
I1 | 0.01390 (9) | 0.01253 (9) | 0.01096 (9) | −0.00020 (5) | 0.00093 (5) | −0.00333 (5) |
Cu1 | 0.01093 (14) | 0.01635 (16) | 0.01184 (15) | −0.00100 (11) | −0.00207 (11) | −0.00041 (11) |
N1 | 0.0102 (10) | 0.0137 (10) | 0.0112 (10) | −0.0001 (7) | 0.0004 (7) | 0.0003 (8) |
C1 | 0.0131 (12) | 0.0163 (12) | 0.0227 (13) | 0.0028 (9) | −0.0012 (10) | −0.0040 (10) |
C3 | 0.0108 (11) | 0.0230 (14) | 0.0209 (13) | −0.0013 (10) | −0.0014 (10) | 0.0002 (11) |
C2 | 0.0121 (11) | 0.0210 (13) | 0.0201 (13) | 0.0016 (9) | −0.0030 (10) | 0.0002 (11) |
C5 | 0.0140 (12) | 0.0157 (12) | 0.0194 (13) | −0.0023 (9) | −0.0025 (10) | 0.0014 (10) |
C4 | 0.0139 (12) | 0.0171 (12) | 0.0220 (13) | −0.0039 (9) | −0.0048 (10) | −0.0003 (10) |
Geometric parameters (Å, º) top
I1—Cu1 | 2.6901 (4) | C3—H3A | 0.9900 |
Cu1—N1 | 2.052 (2) | C3—H3B | 0.9900 |
N1—C1 | 1.482 (3) | C2—H2A | 0.9900 |
N1—C5 | 1.489 (3) | C2—H2B | 0.9900 |
N1—H1 | 1.00 (3) | C5—C4 | 1.527 (4) |
C1—C2 | 1.523 (4) | C5—H5A | 0.9900 |
C1—H1A | 0.9900 | C5—H5B | 0.9900 |
C1—H1B | 0.9900 | C4—H4A | 0.9900 |
C3—C2 | 1.533 (4) | C4—H4B | 0.9900 |
C3—C4 | 1.534 (4) | | |
| | | |
Cu1i—I1—Cu1 | 58.905 (12) | N1—C1—C2 | 113.1 (2) |
Cu1i—I1—Cu1ii | 58.609 (12) | N1—C1—H1A | 109.0 |
Cu1—I1—Cu1ii | 57.444 (12) | C2—C1—H1A | 109.0 |
N1—Cu1—Cu1ii | 142.33 (6) | N1—C1—H1B | 109.0 |
N1—Cu1—Cu1i | 147.18 (6) | C2—C1—H1B | 109.0 |
Cu1ii—Cu1—Cu1i | 60.566 (8) | H1A—C1—H1B | 107.8 |
N1—Cu1—Cu1iii | 144.66 (6) | C2—C3—C4 | 110.1 (2) |
Cu1ii—Cu1—Cu1iii | 60.567 (8) | C2—C3—H3A | 109.7 |
Cu1i—Cu1—Cu1iii | 58.864 (15) | C4—C3—H3A | 109.7 |
N1—Cu1—I1iii | 105.86 (6) | C2—C3—H3B | 109.7 |
Cu1ii—Cu1—I1iii | 111.767 (8) | C4—C3—H3B | 109.7 |
Cu1i—Cu1—I1iii | 61.256 (16) | H3A—C3—H3B | 108.2 |
Cu1iii—Cu1—I1iii | 60.649 (16) | C1—C2—C3 | 111.1 (2) |
N1—Cu1—I1 | 105.16 (6) | C1—C2—H2A | 109.4 |
Cu1ii—Cu1—I1 | 61.748 (12) | C3—C2—H2A | 109.4 |
Cu1i—Cu1—I1 | 60.446 (13) | C1—C2—H2B | 109.4 |
Cu1iii—Cu1—I1 | 110.178 (11) | C3—C2—H2B | 109.4 |
I1iii—Cu1—I1 | 112.842 (12) | H2A—C2—H2B | 108.0 |
N1—Cu1—I1ii | 103.38 (6) | N1—C5—C4 | 112.5 (2) |
Cu1ii—Cu1—I1ii | 60.808 (12) | N1—C5—H5A | 109.1 |
Cu1i—Cu1—I1ii | 109.432 (11) | C4—C5—H5A | 109.1 |
Cu1iii—Cu1—I1ii | 60.133 (13) | N1—C5—H5B | 109.1 |
I1iii—Cu1—I1ii | 112.068 (12) | C4—C5—H5B | 109.1 |
I1—Cu1—I1ii | 116.224 (12) | H5A—C5—H5B | 107.8 |
C1—N1—C5 | 110.9 (2) | C5—C4—C3 | 111.6 (2) |
C1—N1—Cu1 | 112.49 (16) | C5—C4—H4A | 109.3 |
C5—N1—Cu1 | 113.07 (16) | C3—C4—H4A | 109.3 |
C1—N1—H1 | 105.9 (16) | C5—C4—H4B | 109.3 |
C5—N1—H1 | 108.1 (16) | C3—C4—H4B | 109.3 |
Cu1—N1—H1 | 106.0 (17) | H4A—C4—H4B | 108.0 |
| | | |
Cu1i—I1—Cu1—N1 | −147.92 (7) | I1ii—Cu1—N1—C1 | −56.24 (18) |
Cu1ii—I1—Cu1—N1 | 141.75 (6) | Cu1ii—Cu1—N1—C5 | 118.01 (16) |
Cu1i—I1—Cu1—Cu1ii | 70.329 (9) | Cu1i—Cu1—N1—C5 | −3.6 (2) |
Cu1ii—I1—Cu1—Cu1i | −70.329 (9) | Cu1iii—Cu1—N1—C5 | −126.12 (16) |
Cu1i—I1—Cu1—Cu1iii | 32.684 (16) | I1iii—Cu1—N1—C5 | −64.82 (17) |
Cu1ii—I1—Cu1—Cu1iii | −37.645 (18) | I1—Cu1—N1—C5 | 54.85 (18) |
Cu1i—I1—Cu1—I1iii | −32.994 (14) | I1ii—Cu1—N1—C5 | 177.20 (16) |
Cu1ii—I1—Cu1—I1iii | −103.324 (11) | C5—N1—C1—C2 | −55.6 (3) |
Cu1i—I1—Cu1—I1ii | 98.454 (14) | Cu1—N1—C1—C2 | 176.64 (18) |
Cu1ii—I1—Cu1—I1ii | 28.125 (16) | N1—C1—C2—C3 | 55.4 (3) |
Cu1ii—Cu1—N1—C1 | −115.43 (17) | C4—C3—C2—C1 | −53.1 (3) |
Cu1i—Cu1—N1—C1 | 122.93 (16) | C1—N1—C5—C4 | 55.1 (3) |
Cu1iii—Cu1—N1—C1 | 0.4 (2) | Cu1—N1—C5—C4 | −177.54 (18) |
I1iii—Cu1—N1—C1 | 61.74 (18) | N1—C5—C4—C3 | −54.8 (3) |
I1—Cu1—N1—C1 | −178.58 (16) | C2—C3—C4—C5 | 53.1 (3) |
Symmetry codes: (i) −y+3/2, x, −z+1/2; (ii) −x+3/2, −y+3/2, z; (iii) y, −x+3/2, −z+1/2. |
Experimental details
Crystal data |
Chemical formula | C20H44Cu4I4N4 |
Mr | 1102.39 |
Crystal system, space group | Tetragonal, P42/n |
Temperature (K) | 90 |
a, c (Å) | 14.6049 (12), 7.5464 (12) |
V (Å3) | 1609.7 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 6.46 |
Crystal size (mm) | 0.10 × 0.02 × 0.02 |
|
Data collection |
Diffractometer | Bruker SMART APEXII CCD diffractometer |
Absorption correction | Multi-scan Absorption correction done by SORTAV
Blessing, R. H.: (1995) Acta Cryst. A51, 33-38 |
Tmin, Tmax | 0.589, 1.155 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 33915, 2460, 2056 |
Rint | 0.077 |
(sin θ/λ)max (Å−1) | 0.715 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.024, 0.060, 1.11 |
No. of reflections | 2460 |
No. of parameters | 77 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.60, −1.51 |
Subscribe to Journal of Synchrotron Radiation
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.