Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804011912/ob6366sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804011912/ob6366Isup2.hkl |
CCDC reference: 242283
Data collection: SMART-W2K/NT (Bruker, 2003); cell refinement: SMART-W2K/NT; data reduction: SAINT-W2K/NT (Bruker, 2003); program(s) used to solve structure: SHELXTL-NT (Bruker, 2003); program(s) used to refine structure: SHELXTL-NT; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL-NT.
[Cr(C15H12N4)(H2O)3](CF3SO3)3 | Dx = 1.721 Mg m−3 |
Mr = 801.54 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3 | Cell parameters from 8816 reflections |
Hall symbol: -P 3 | θ = 2.7–28.3° |
a = 13.0562 (3) Å | µ = 0.69 mm−1 |
c = 10.4754 (5) Å | T = 173 K |
V = 1546.45 (9) Å3 | Block, red |
Z = 2 | 0.52 × 0.51 × 0.32 mm |
F(000) = 806 |
Bruker SMART APEX CCD area-detector diffractometer | 2563 independent reflections |
Radiation source: fine-focus sealed tube | 2413 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
Detector resolution: 8.366 pixels mm-1 | θmax = 28.3°, θmin = 1.8° |
φ and ω scans | h = −11→17 |
Absorption correction: multi-scan (SADABS; Scheldrick, 1996) | k = −17→13 |
Tmin = 0.716, Tmax = 0.810 | l = −13→13 |
11598 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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.089 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0476P)2 + 0.7758P] where P = (Fo2 + 2Fc2)/3 |
2563 reflections | (Δ/σ)max = 0.001 |
150 parameters | Δρmax = 0.35 e Å−3 |
0 restraints | Δρmin = −0.47 e Å−3 |
Experimental. none |
Geometry. Angle with sdev 52.10(0.03) N1—Cr1—N2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 10.8598 (0.0048) x + 0.8404 (0.0085) y - 0.2617 (0.0070) z = 7.3043 (0.0059) * 0.0020 (0.0009) N1 * -0.0048 (0.0010) C1 * 0.0026 (0.0011) C2 * 0.0022 (0.0012) C3 * -0.0049 (0.0012) C4 * 0.0029 (0.0011) C5 Rms deviation of fitted atoms = 0.0034 |
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 | ||
Cr1 | 0.6667 | 0.3333 | 0.61522 (3) | 0.01738 (11) | |
N1 | 0.65562 (10) | 0.45075 (10) | 0.73486 (11) | 0.0205 (2) | |
N2 | 0.6667 | 0.3333 | 0.90160 (19) | 0.0209 (4) | |
O1 | 0.78024 (10) | 0.46132 (10) | 0.50174 (11) | 0.0244 (2) | |
C1 | 0.65926 (12) | 0.43497 (12) | 0.86158 (13) | 0.0211 (3) | |
C2 | 0.65618 (14) | 0.51100 (14) | 0.95036 (14) | 0.0285 (3) | |
C3 | 0.64762 (16) | 0.60705 (15) | 0.90668 (16) | 0.0339 (3) | |
C4 | 0.64271 (16) | 0.62306 (14) | 0.77688 (17) | 0.0323 (3) | |
C5 | 0.64748 (13) | 0.54401 (13) | 0.69335 (14) | 0.0261 (3) | |
H2 | 0.6598 | 0.4982 | 1.0391 | 0.034* | |
H3 | 0.6452 | 0.6612 | 0.9655 | 0.041* | |
H4 | 0.6361 | 0.6878 | 0.7456 | 0.039* | |
H5 | 0.6450 | 0.5556 | 0.6041 | 0.031* | |
H10 | 0.836 (3) | 0.506 (2) | 0.524 (3) | 0.051 (8)* | |
H11 | 0.759 (2) | 0.483 (2) | 0.442 (2) | 0.040 (6)* | |
C6 | 0.81468 (19) | 0.78434 (19) | 0.2965 (3) | 0.0517 (5) | |
F1 | 0.87054 (13) | 0.79432 (16) | 0.18730 (17) | 0.0768 (5) | |
F2 | 0.88681 (13) | 0.79619 (17) | 0.39179 (19) | 0.0835 (5) | |
F3 | 0.78838 (17) | 0.86921 (13) | 0.3048 (3) | 0.0997 (7) | |
S2 | 0.68084 (3) | 0.64109 (3) | 0.30528 (3) | 0.02578 (11) | |
O2 | 0.63078 (12) | 0.64370 (15) | 0.42784 (12) | 0.0442 (3) | |
O3 | 0.72438 (12) | 0.55845 (11) | 0.30167 (12) | 0.0378 (3) | |
O4 | 0.61319 (11) | 0.63906 (13) | 0.19726 (11) | 0.0390 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr1 | 0.01827 (13) | 0.01827 (13) | 0.01560 (18) | 0.00914 (7) | 0.000 | 0.000 |
N1 | 0.0215 (5) | 0.0201 (5) | 0.0200 (5) | 0.0106 (4) | 0.0008 (4) | −0.0002 (4) |
N2 | 0.0215 (6) | 0.0215 (6) | 0.0198 (9) | 0.0108 (3) | 0.000 | 0.000 |
O1 | 0.0223 (5) | 0.0241 (5) | 0.0220 (5) | 0.0080 (4) | 0.0000 (4) | 0.0034 (4) |
C1 | 0.0201 (6) | 0.0211 (6) | 0.0215 (6) | 0.0097 (5) | 0.0007 (5) | −0.0004 (5) |
C2 | 0.0335 (7) | 0.0283 (7) | 0.0235 (7) | 0.0155 (6) | 0.0010 (5) | −0.0039 (5) |
C3 | 0.0436 (9) | 0.0283 (7) | 0.0337 (8) | 0.0210 (7) | 0.0016 (7) | −0.0072 (6) |
C4 | 0.0400 (8) | 0.0244 (7) | 0.0368 (8) | 0.0194 (7) | 0.0018 (7) | 0.0004 (6) |
C5 | 0.0303 (7) | 0.0235 (6) | 0.0261 (7) | 0.0146 (6) | 0.0012 (5) | 0.0024 (5) |
C6 | 0.0363 (9) | 0.0365 (10) | 0.0792 (15) | 0.0161 (8) | −0.0052 (10) | −0.0017 (10) |
F1 | 0.0454 (7) | 0.0769 (10) | 0.0957 (12) | 0.0214 (7) | 0.0281 (8) | 0.0416 (9) |
F2 | 0.0426 (8) | 0.0868 (12) | 0.1038 (13) | 0.0194 (8) | −0.0329 (8) | −0.0285 (10) |
F3 | 0.0803 (12) | 0.0348 (7) | 0.185 (2) | 0.0294 (8) | −0.0098 (13) | −0.0089 (10) |
S2 | 0.02477 (18) | 0.0332 (2) | 0.02258 (19) | 0.01688 (15) | 0.00129 (12) | 0.00198 (13) |
O2 | 0.0474 (8) | 0.0816 (10) | 0.0247 (6) | 0.0480 (8) | 0.0050 (5) | 0.0057 (6) |
O3 | 0.0471 (7) | 0.0399 (7) | 0.0372 (6) | 0.0298 (6) | 0.0073 (5) | 0.0072 (5) |
O4 | 0.0353 (6) | 0.0563 (8) | 0.0273 (6) | 0.0242 (6) | −0.0041 (5) | 0.0015 (5) |
Cr1—O1i | 1.9815 (11) | N2—C1i | 1.4402 (15) |
Cr1—O1ii | 1.9815 (11) | N2—C1ii | 1.4402 (15) |
Cr1—O1 | 1.9815 (11) | N2—C1 | 1.4402 (15) |
Cr1—N1ii | 2.0403 (12) | C1—C2 | 1.375 (2) |
Cr1—N1i | 2.0403 (12) | C5—C4 | 1.378 (2) |
Cr1—N1 | 2.0403 (12) | C5—H5 | 0.9500 |
S2—O4 | 1.4274 (12) | C2—C3 | 1.391 (2) |
S2—O2 | 1.4487 (12) | C2—H2 | 0.9500 |
S2—O3 | 1.4500 (12) | C4—C3 | 1.382 (2) |
S2—C6 | 1.814 (2) | C4—H4 | 0.9500 |
O1—H10 | 0.71 (3) | C3—H3 | 0.9500 |
O1—H11 | 0.79 (3) | F1—C6 | 1.327 (3) |
N1—C5 | 1.3461 (18) | F2—C6 | 1.328 (3) |
N1—C1 | 1.3478 (18) | F3—C6 | 1.317 (3) |
O1i—Cr1—O1ii | 87.71 (5) | C1—N1—Cr1 | 117.96 (9) |
O1i—Cr1—O1 | 87.71 (5) | C1i—N2—C1ii | 111.90 (8) |
O1ii—Cr1—O1 | 87.71 (5) | C1i—N2—C1 | 111.90 (8) |
O1i—Cr1—N1ii | 178.45 (5) | C1ii—N2—C1 | 111.89 (8) |
O1ii—Cr1—N1ii | 92.24 (5) | N1—C1—C2 | 122.65 (13) |
O1—Cr1—N1ii | 93.83 (5) | N1—C1—N2 | 116.83 (13) |
O1i—Cr1—N1i | 92.24 (5) | C2—C1—N2 | 120.52 (14) |
O1ii—Cr1—N1i | 93.83 (5) | N1—C5—C4 | 121.73 (14) |
O1—Cr1—N1i | 178.45 (5) | N1—C5—H5 | 119.1 |
N1ii—Cr1—N1i | 86.22 (5) | C4—C5—H5 | 119.1 |
O1i—Cr1—N1 | 93.83 (5) | C1—C2—C3 | 118.22 (14) |
O1ii—Cr1—N1 | 178.45 (5) | C1—C2—H2 | 120.9 |
O1—Cr1—N1 | 92.24 (5) | C3—C2—H2 | 120.9 |
N1ii—Cr1—N1 | 86.22 (5) | C5—C4—C3 | 119.25 (14) |
N1i—Cr1—N1 | 86.22 (5) | C5—C4—H4 | 120.4 |
O4—S2—O2 | 114.88 (8) | C3—C4—H4 | 120.4 |
O4—S2—O3 | 115.76 (8) | C4—C3—C2 | 119.38 (14) |
O2—S2—O3 | 112.95 (8) | C4—C3—H3 | 120.3 |
O4—S2—C6 | 104.29 (10) | C2—C3—H3 | 120.3 |
O2—S2—C6 | 103.54 (11) | F3—C6—F1 | 109.6 (2) |
O3—S2—C6 | 103.41 (9) | F3—C6—F2 | 108.7 (2) |
Cr1—O1—H10 | 122 (2) | F1—C6—F2 | 108.29 (19) |
Cr1—O1—H11 | 122.1 (17) | F3—C6—S2 | 110.00 (16) |
H10—O1—H11 | 111 (3) | F1—C6—S2 | 110.11 (16) |
C5—N1—C1 | 118.77 (12) | F2—C6—S2 | 110.08 (17) |
C5—N1—Cr1 | 123.26 (10) | ||
O1i—Cr1—N1—C5 | −45.13 (12) | C1—N1—C5—C4 | −0.1 (2) |
O1—Cr1—N1—C5 | 42.73 (12) | Cr1—N1—C5—C4 | −178.59 (12) |
N1ii—Cr1—N1—C5 | 136.42 (13) | N1—C1—C2—C3 | 0.7 (2) |
N1i—Cr1—N1—C5 | −137.12 (13) | N2—C1—C2—C3 | −179.26 (13) |
O1i—Cr1—N1—C1 | 136.34 (10) | N1—C5—C4—C3 | 0.7 (3) |
O1—Cr1—N1—C1 | −135.80 (10) | C5—C4—C3—C2 | −0.6 (3) |
N1ii—Cr1—N1—C1 | −42.11 (8) | C1—C2—C3—C4 | −0.1 (3) |
N1i—Cr1—N1—C1 | 44.35 (8) | O4—S2—C6—F3 | 61.4 (2) |
C5—N1—C1—C2 | −0.7 (2) | O2—S2—C6—F3 | −59.1 (2) |
Cr1—N1—C1—C2 | 177.94 (11) | O3—S2—C6—F3 | −177.11 (19) |
C5—N1—C1—N2 | 179.34 (11) | O4—S2—C6—F1 | −59.52 (17) |
Cr1—N1—C1—N2 | −2.06 (15) | O2—S2—C6—F1 | 179.95 (14) |
C1i—N2—C1—N1 | −61.95 (16) | O3—S2—C6—F1 | 61.94 (17) |
C1ii—N2—C1—N1 | 64.54 (15) | O4—S2—C6—F2 | −178.84 (16) |
C1i—N2—C1—C2 | 118.05 (18) | O2—S2—C6—F2 | 60.64 (18) |
C1ii—N2—C1—C2 | −115.46 (18) | O3—S2—C6—F2 | −57.38 (18) |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H10···O2iii | 0.71 (3) | 1.89 (3) | 2.5995 (17) | 176 (3) |
O1—H11···O3 | 0.79 (3) | 1.94 (3) | 2.7308 (17) | 172 (2) |
Symmetry code: (iii) x−y+1, x, −z+1. |