Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804015016/tk6168sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804015016/tk6168Isup2.hkl |
CCDC reference: 248737
Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994).; cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995).; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997).; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997).; software used to prepare material for publication: WinGX (Farrugia, 1999)..
[Re(C5H5N)(C10H8N2)(CO)3](CF3O3S) | F(000) = 2512 |
Mr = 654.58 | Dx = 2.121 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -p 2ac 2ab | Cell parameters from 24 reflections |
a = 12.178 (2) Å | θ = 10–12° |
b = 14.414 (3) Å | µ = 6.10 mm−1 |
c = 23.357 (5) Å | T = 100 K |
V = 4100.1 (14) Å3 | Needle, green–yellow |
Z = 8 | 0.38 × 0.15 × 0.08 mm |
Enraf–Nonius CAD-4 diffractometer | Rint = 0 |
non–profiled ω/2θ scans | θmax = 25.0°, θmin = 1.7° |
Absorption correction: ψ scan North, Phillips & Mathews (1968) | h = 0→14 |
Tmin = 0.505, Tmax = 0.612 | k = 0→17 |
3601 measured reflections | l = 0→27 |
3601 independent reflections | 3 standard reflections every 60 min |
2357 reflections with I > 2σ(I) | intensity decay: none |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.033 | w = 1/[σ2(Fo2) + (0.0313P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.074 | (Δ/σ)max = 0.001 |
S = 1.03 | Δρmax = 1.01 e Å−3 |
3601 reflections | Δρmin = −0.74 e Å−3 |
298 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. |
x | y | z | Uiso*/Ueq | ||
Re | 0.237095 (18) | 0.828579 (19) | 0.334964 (11) | 0.01160 (9) | |
S1 | 0.26244 (16) | 0.28566 (13) | 0.57860 (8) | 0.0184 (4) | |
O1 | 0.0372 (4) | 0.8173 (4) | 0.2555 (2) | 0.0219 (12) | |
O3 | 0.1465 (4) | 0.6677 (4) | 0.4072 (2) | 0.0218 (12) | |
O4 | 0.2120 (5) | 0.3763 (4) | 0.5805 (2) | 0.0300 (15) | |
N3 | 0.1639 (5) | 0.9390 (4) | 0.3872 (3) | 0.0128 (15) | |
O2 | 0.3528 (4) | 0.6731 (4) | 0.2679 (2) | 0.0188 (11) | |
N1 | 0.3817 (5) | 0.8712 (5) | 0.3828 (3) | 0.0162 (15) | |
N2 | 0.3093 (5) | 0.9400 (4) | 0.2860 (2) | 0.0124 (14) | |
F3 | 0.1897 (4) | 0.1221 (4) | 0.6089 (2) | 0.0414 (15) | |
F2 | 0.1277 (4) | 0.2342 (4) | 0.6595 (2) | 0.0520 (16) | |
C2 | 0.3099 (6) | 0.7327 (6) | 0.2926 (3) | 0.0149 (17) | |
C4 | 0.4135 (6) | 0.8308 (6) | 0.4329 (3) | 0.0177 (16) | |
H4 | 0.3735 | 0.779 | 0.4469 | 0.021* | |
C3 | 0.1806 (6) | 0.7301 (6) | 0.3812 (3) | 0.0154 (17) | |
F1 | 0.0652 (4) | 0.2120 (4) | 0.5745 (2) | 0.0399 (14) | |
C6 | 0.5590 (6) | 0.9394 (6) | 0.4443 (4) | 0.0197 (19) | |
H6 | 0.6201 | 0.9629 | 0.4651 | 0.024* | |
C19 | 0.1559 (7) | 0.2103 (7) | 0.6066 (4) | 0.027 (2) | |
C13 | 0.2729 (6) | 0.9680 (5) | 0.2347 (3) | 0.0171 (16) | |
H13 | 0.2149 | 0.9348 | 0.2169 | 0.021* | |
C1 | 0.1101 (6) | 0.8187 (6) | 0.2860 (3) | 0.0178 (17) | |
C15 | 0.1378 (6) | 1.0102 (6) | 0.4792 (3) | 0.0198 (18) | |
H15 | 0.151 | 1.0094 | 0.5193 | 0.024* | |
C18 | 0.1082 (5) | 1.0103 (6) | 0.3650 (3) | 0.0177 (18) | |
H18 | 0.0977 | 1.0112 | 0.3247 | 0.021* | |
C14 | 0.1770 (6) | 0.9395 (5) | 0.4448 (3) | 0.0180 (18) | |
H14 | 0.2147 | 0.8893 | 0.4623 | 0.022* | |
C16 | 0.0798 (6) | 1.0814 (6) | 0.4550 (3) | 0.0204 (19) | |
H16 | 0.0502 | 1.1293 | 0.4783 | 0.025* | |
C9 | 0.3956 (6) | 0.9841 (6) | 0.3100 (3) | 0.0187 (18) | |
C8 | 0.4369 (6) | 0.9447 (6) | 0.3642 (4) | 0.0177 (19) | |
C7 | 0.5254 (6) | 0.9813 (6) | 0.3935 (3) | 0.0207 (18) | |
H7 | 0.5628 | 1.0344 | 0.3793 | 0.025* | |
C5 | 0.5021 (6) | 0.8632 (6) | 0.4639 (3) | 0.0222 (19) | |
H5 | 0.5236 | 0.8332 | 0.4984 | 0.027* | |
C10 | 0.4414 (6) | 1.0616 (5) | 0.2839 (3) | 0.0180 (18) | |
H10 | 0.5002 | 1.0937 | 0.3019 | 0.022* | |
C12 | 0.3172 (6) | 1.0436 (5) | 0.2071 (3) | 0.0165 (17) | |
H12 | 0.2892 | 1.0622 | 0.1709 | 0.02* | |
C11 | 0.4014 (7) | 1.0919 (5) | 0.2318 (3) | 0.023 (2) | |
H11 | 0.4317 | 1.145 | 0.2136 | 0.028* | |
C17 | 0.0646 (6) | 1.0831 (6) | 0.3965 (4) | 0.0200 (18) | |
H17 | 0.0258 | 1.1323 | 0.3784 | 0.024* | |
O6 | 0.3522 (4) | 0.2732 (4) | 0.6177 (2) | 0.0257 (14) | |
O5 | 0.2795 (4) | 0.2492 (4) | 0.5216 (2) | 0.0254 (13) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re | 0.01091 (13) | 0.01109 (14) | 0.01280 (14) | −0.00084 (13) | 0.00098 (13) | 0.00042 (15) |
S1 | 0.0191 (10) | 0.0175 (9) | 0.0188 (9) | 0.0016 (9) | 0.0023 (9) | −0.0019 (8) |
O1 | 0.015 (3) | 0.025 (3) | 0.025 (3) | −0.009 (2) | −0.006 (2) | −0.002 (3) |
O3 | 0.027 (3) | 0.019 (3) | 0.019 (3) | −0.005 (3) | 0.002 (2) | −0.003 (3) |
O4 | 0.031 (3) | 0.024 (3) | 0.035 (4) | 0.007 (3) | −0.005 (3) | −0.007 (3) |
N3 | 0.013 (3) | 0.014 (4) | 0.012 (4) | 0.002 (3) | −0.002 (3) | 0.000 (3) |
O2 | 0.019 (3) | 0.018 (3) | 0.018 (3) | 0.006 (3) | 0.003 (2) | −0.001 (3) |
N1 | 0.012 (3) | 0.019 (4) | 0.017 (4) | 0.008 (3) | 0.001 (3) | −0.005 (3) |
N2 | 0.014 (3) | 0.014 (4) | 0.009 (3) | −0.003 (3) | 0.004 (3) | −0.002 (3) |
F3 | 0.059 (4) | 0.030 (3) | 0.035 (3) | −0.014 (3) | −0.003 (3) | 0.011 (3) |
F2 | 0.060 (3) | 0.075 (5) | 0.021 (3) | −0.022 (3) | 0.024 (3) | −0.016 (3) |
C2 | 0.012 (4) | 0.020 (5) | 0.013 (4) | −0.005 (3) | −0.001 (3) | 0.008 (4) |
C4 | 0.018 (4) | 0.021 (4) | 0.015 (4) | 0.007 (4) | 0.001 (3) | −0.007 (4) |
C3 | 0.016 (4) | 0.013 (4) | 0.017 (4) | 0.002 (3) | 0.007 (3) | −0.001 (4) |
F1 | 0.025 (3) | 0.055 (4) | 0.040 (3) | −0.006 (2) | 0.001 (2) | −0.010 (3) |
C6 | 0.005 (3) | 0.027 (5) | 0.028 (5) | 0.000 (3) | −0.004 (3) | −0.003 (4) |
C19 | 0.030 (5) | 0.037 (6) | 0.015 (5) | −0.004 (4) | 0.003 (4) | −0.005 (4) |
C13 | 0.020 (4) | 0.011 (4) | 0.021 (4) | −0.002 (3) | 0.002 (3) | −0.001 (3) |
C1 | 0.009 (3) | 0.017 (4) | 0.027 (5) | 0.001 (3) | 0.006 (3) | −0.002 (4) |
C15 | 0.022 (4) | 0.026 (5) | 0.011 (4) | −0.001 (4) | 0.003 (3) | −0.004 (4) |
C18 | 0.012 (4) | 0.020 (5) | 0.021 (5) | −0.002 (3) | −0.006 (3) | 0.002 (4) |
C14 | 0.024 (4) | 0.014 (5) | 0.017 (4) | 0.003 (3) | 0.006 (3) | 0.001 (4) |
C16 | 0.022 (4) | 0.022 (5) | 0.017 (4) | −0.002 (4) | 0.007 (3) | −0.011 (4) |
C9 | 0.018 (4) | 0.018 (5) | 0.021 (4) | 0.004 (3) | 0.003 (3) | 0.002 (4) |
C8 | 0.009 (4) | 0.019 (5) | 0.025 (5) | −0.006 (3) | 0.003 (3) | 0.000 (4) |
C7 | 0.022 (4) | 0.019 (5) | 0.021 (4) | 0.001 (4) | 0.006 (3) | −0.005 (4) |
C5 | 0.018 (4) | 0.024 (5) | 0.024 (5) | 0.015 (3) | −0.003 (3) | −0.001 (4) |
C10 | 0.020 (4) | 0.014 (4) | 0.020 (5) | −0.005 (3) | 0.007 (3) | −0.001 (4) |
C12 | 0.021 (4) | 0.017 (4) | 0.012 (4) | 0.004 (3) | 0.005 (3) | 0.000 (3) |
C11 | 0.035 (5) | 0.007 (4) | 0.027 (5) | 0.000 (3) | 0.012 (4) | 0.000 (4) |
C17 | 0.022 (4) | 0.011 (4) | 0.028 (5) | −0.001 (3) | 0.004 (4) | −0.001 (4) |
O6 | 0.015 (3) | 0.030 (4) | 0.032 (4) | 0.001 (2) | −0.009 (2) | −0.004 (3) |
O5 | 0.036 (3) | 0.027 (3) | 0.014 (3) | 0.001 (3) | 0.007 (2) | −0.003 (3) |
Re—N1 | 2.174 (6) | C6—C5 | 1.377 (11) |
Re—N2 | 2.158 (6) | C6—C7 | 1.393 (11) |
Re—N3 | 2.194 (6) | C6—H6 | 0.95 |
Re—C1 | 1.929 (7) | C13—C12 | 1.375 (10) |
Re—C2 | 1.918 (8) | C13—H13 | 0.95 |
Re—C3 | 1.912 (8) | C15—C16 | 1.368 (11) |
S1—O6 | 1.435 (5) | C15—C14 | 1.382 (10) |
S1—O4 | 1.444 (6) | C15—H15 | 0.95 |
S1—O5 | 1.446 (5) | C18—C17 | 1.387 (11) |
S1—C19 | 1.815 (9) | C18—H18 | 0.95 |
O1—C1 | 1.139 (9) | C14—H14 | 0.95 |
O3—C3 | 1.162 (9) | C16—C17 | 1.380 (11) |
N3—C18 | 1.335 (9) | C16—H16 | 0.95 |
N3—C14 | 1.357 (9) | C9—C10 | 1.390 (11) |
O2—C2 | 1.158 (9) | C9—C8 | 1.476 (11) |
N1—C8 | 1.328 (10) | C8—C7 | 1.382 (11) |
N1—C4 | 1.362 (9) | C7—H7 | 0.95 |
N2—C13 | 1.341 (9) | C5—H5 | 0.95 |
N2—C9 | 1.349 (9) | C10—C11 | 1.383 (11) |
F3—C19 | 1.337 (11) | C10—H10 | 0.95 |
F2—C19 | 1.327 (9) | C12—C11 | 1.368 (11) |
C4—C5 | 1.381 (10) | C12—H12 | 0.95 |
C4—H4 | 0.95 | C11—H11 | 0.95 |
F1—C19 | 1.335 (10) | C17—H17 | 0.95 |
N1—Re—N2 | 74.5 (2) | F1—C19—S1 | 112.2 (6) |
N1—Re—N3 | 80.7 (2) | F3—C19—S1 | 111.3 (6) |
N1—Re—C1 | 167.2 (3) | N2—C13—C12 | 121.9 (7) |
N1—Re—C2 | 95.4 (3) | N2—C13—H13 | 119 |
N1—Re—C3 | 102.2 (3) | C12—C13—H13 | 119 |
N2—Re—N3 | 85.4 (2) | O1—C1—Re | 176.1 (7) |
N2—Re—C1 | 93.9 (3) | C16—C15—C14 | 119.5 (7) |
N2—Re—C2 | 94.3 (2) | C16—C15—H15 | 120.3 |
N2—Re—C3 | 176.6 (3) | C14—C15—H15 | 120.3 |
N3—Re—C1 | 93.3 (3) | N3—C18—C17 | 124.9 (8) |
N3—Re—C2 | 176.1 (3) | N3—C18—H18 | 117.5 |
N3—Re—C3 | 94.5 (3) | C17—C18—H18 | 117.5 |
C1—Re—C2 | 90.7 (3) | N3—C14—C15 | 122.7 (7) |
C1—Re—C3 | 89.5 (3) | N3—C14—H14 | 118.7 |
C2—Re—C3 | 85.6 (3) | C15—C14—H14 | 118.7 |
O6—S1—O4 | 114.7 (4) | C15—C16—C17 | 119.4 (8) |
O6—S1—O5 | 115.5 (3) | C15—C16—H16 | 120.3 |
O4—S1—O5 | 114.7 (3) | C17—C16—H16 | 120.3 |
O6—S1—C19 | 103.9 (4) | N2—C9—C10 | 120.6 (7) |
O4—S1—C19 | 103.1 (4) | N2—C9—C8 | 116.1 (7) |
O5—S1—C19 | 102.5 (4) | C10—C9—C8 | 123.3 (7) |
C18—N3—C14 | 116.1 (7) | N1—C8—C7 | 122.5 (8) |
C18—N3—Re | 123.3 (5) | N1—C8—C9 | 114.5 (7) |
C14—N3—Re | 120.5 (5) | C7—C8—C9 | 122.9 (7) |
C8—N1—C4 | 118.5 (7) | C8—C7—C6 | 119.0 (8) |
C8—N1—Re | 117.9 (5) | C8—C7—H7 | 120.5 |
C4—N1—Re | 123.4 (5) | C6—C7—H7 | 120.5 |
C13—N2—C9 | 119.1 (6) | C6—C5—C4 | 119.2 (8) |
C13—N2—Re1 | 124.3 (5) | C6—C5—H5 | 120.4 |
C9—N2—Re | 116.6 (5) | C4—C5—H5 | 120.4 |
O2—C2—Re | 178.3 (7) | C11—C10—C9 | 119.9 (8) |
N1—C4—C5 | 121.9 (8) | C11—C10—H10 | 120 |
N1—C4—H4 | 119 | C9—C10—H10 | 120 |
C5—C4—H4 | 119 | C11—C12—C13 | 120.0 (7) |
O3—C3—Re | 176.9 (7) | C11—C12—H12 | 120 |
C5—C6—C7 | 118.8 (7) | C13—C12—H12 | 120 |
C5—C6—H6 | 120.6 | C12—C11—C10 | 118.3 (7) |
C7—C6—H6 | 120.6 | C12—C11—H11 | 120.8 |
F2—C19—F1 | 107.7 (7) | C10—C11—H11 | 120.8 |
F2—C19—F3 | 106.9 (8) | C16—C17—C18 | 117.4 (8) |
F1—C19—F3 | 107.1 (7) | C16—C17—H17 | 121.3 |
F2—C19—S1 | 111.4 (6) | C18—C17—H17 | 121.3 |