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
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.011 Å
- R factor = 0.033
- wR factor = 0.074
- Data-to-parameter ratio = 12.1
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT052_ALERT_1_A (Proper) Absorption Correction Method Missing .. ? PLAT057_ALERT_3_A Correction for Absorption Required RT(exp) ... 1.77
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.505 0.612 Tmin and Tmax expected: 0.345 0.614 RR = 1.468 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11 PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. O2 .. 2.87 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact F2 .. O1 .. 2.92 Ang. PLAT712_ALERT_1_C ANGLE Unknown or Inconsistent Label .......... RE1 C13 N2 RE1
2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 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
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 |