Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807016996/tk2147sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807016996/tk2147Isup2.hkl |
CCDC reference: 647458
Key indicators
- Single-crystal X-ray study
- T = 110 K
- Mean (C-C) = 0.014 Å
- R factor = 0.058
- wR factor = 0.151
- Data-to-parameter ratio = 16.3
checkCIF/PLATON results
No syntax errors found
Alert level A PLAT355_ALERT_3_A Long O-H Bond (0.82A) O5 - H5O ... 1.13 Ang.
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.308 0.907 Tmin and Tmax expected: 0.276 0.915 RR = 1.127 Please check that your absorption correction is appropriate. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.13 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.09 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.73 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Re1 - C1 .. 5.80 su PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C1S PLAT309_ALERT_2_C Single Bonded Oxygen (C-O .GT. 1.3 Ang) ........ O4 PLAT309_ALERT_2_C Single Bonded Oxygen (C-O .GT. 1.3 Ang) ........ O6 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 14 PLAT355_ALERT_3_C Long O-H Bond (0.82A) O7 - H7O ... 1.06 Ang. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 35.00 A 3
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 7 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
[ReCl(C10H11NO2)2(CO)3]·CHCl3 | F(000) = 1520 |
Mr = 779.44 | Dx = 1.726 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8612 reflections |
a = 10.889 (4) Å | θ = 2.5–26.0° |
b = 11.607 (4) Å | µ = 4.45 mm−1 |
c = 24.306 (10) Å | T = 110 K |
β = 102.477 (14)° | Plate, colorless |
V = 3000 (2) Å3 | 0.30 × 0.25 × 0.02 mm |
Z = 4 |
Nonius KappaCCD (with Oxford Cryostream) diffractometer | 5749 independent reflections |
Radiation source: fine-focus sealed tube | 4148 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.071 |
ω scans with κ offsets | θmax = 26.0°, θmin = 2.6° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | h = −13→13 |
Tmin = 0.308, Tmax = 0.907 | k = −14→14 |
27300 measured reflections | l = −29→29 |
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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.151 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.37 | w = 1/[σ2(Fo2) + (0.0586P)2 + 2.57P] where P = (Fo2 + 2Fc2)/3 |
5749 reflections | (Δ/σ)max = 0.008 |
353 parameters | Δρmax = 1.97 e Å−3 |
0 restraints | Δρmin = −1.80 e Å−3 |
Experimental. 1H NMR (250 MHz, acetone-d6): 17.08 (s, 2H), 8.84 (d, 4H, J = 6.2), 7.54 (d, 4H, J = 6.3), 1.95 (s, 12H). |
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 | ||
Re1 | 0.38042 (4) | 0.62880 (3) | 0.297709 (14) | 0.03423 (15) | |
Cl1 | 0.4886 (3) | 0.81552 (19) | 0.31775 (9) | 0.0452 (6) | |
O1 | 0.2549 (7) | 0.3933 (6) | 0.2683 (3) | 0.0484 (18) | |
O2 | 0.3017 (8) | 0.6311 (5) | 0.4118 (3) | 0.056 (2) | |
O3 | 0.1247 (8) | 0.7359 (7) | 0.2449 (3) | 0.068 (2) | |
O4 | 0.6907 (7) | 0.5455 (5) | 0.0010 (3) | 0.0473 (18) | |
O5 | 0.6508 (7) | 0.7541 (6) | −0.0046 (3) | 0.0433 (17) | |
H5O | 0.672 (10) | 0.664 (9) | −0.018 (4) | 0.065* | |
O6 | 1.1297 (8) | 0.3703 (7) | 0.4053 (4) | 0.073 (2) | |
O7 | 1.0437 (9) | 0.2884 (8) | 0.4836 (3) | 0.074 (2) | |
H7O | 1.102 (14) | 0.338 (12) | 0.463 (6) | 0.111* | |
N1 | 0.4579 (8) | 0.6302 (6) | 0.2197 (3) | 0.0355 (18) | |
N2 | 0.5625 (7) | 0.5502 (6) | 0.3366 (3) | 0.0340 (18) | |
C1 | 0.3013 (10) | 0.4786 (10) | 0.2791 (4) | 0.043 (3) | |
C2 | 0.3286 (12) | 0.6298 (7) | 0.3675 (4) | 0.051 (3) | |
C3 | 0.2215 (11) | 0.6978 (8) | 0.2652 (4) | 0.046 (3) | |
C4 | 0.5719 (10) | 0.6674 (7) | 0.2197 (4) | 0.036 (2) | |
H4 | 0.6231 | 0.6932 | 0.2543 | 0.044* | |
C5 | 0.6212 (10) | 0.6707 (8) | 0.1712 (4) | 0.039 (2) | |
H5 | 0.7044 | 0.6975 | 0.1732 | 0.046* | |
C6 | 0.5483 (9) | 0.6350 (7) | 0.1206 (3) | 0.033 (2) | |
C7 | 0.4262 (10) | 0.6003 (7) | 0.1203 (3) | 0.035 (2) | |
H7 | 0.3719 | 0.5780 | 0.0859 | 0.042* | |
C8 | 0.3833 (9) | 0.5982 (7) | 0.1699 (3) | 0.034 (2) | |
H8 | 0.2996 | 0.5738 | 0.1690 | 0.041* | |
C9 | 0.6380 (11) | 0.4245 (8) | 0.0714 (4) | 0.048 (3) | |
H9A | 0.6502 | 0.3650 | 0.0445 | 0.072* | |
H9B | 0.5561 | 0.4135 | 0.0812 | 0.072* | |
H9C | 0.7048 | 0.4186 | 0.1055 | 0.072* | |
C10 | 0.6423 (10) | 0.5410 (8) | 0.0455 (4) | 0.040 (2) | |
C11 | 0.5980 (9) | 0.6418 (7) | 0.0673 (3) | 0.033 (2) | |
C12 | 0.6035 (9) | 0.7476 (7) | 0.0401 (3) | 0.034 (2) | |
C13 | 0.5524 (10) | 0.8569 (7) | 0.0582 (4) | 0.045 (2) | |
H13A | 0.6192 | 0.9150 | 0.0658 | 0.067* | |
H13B | 0.5210 | 0.8431 | 0.0925 | 0.067* | |
H13C | 0.4835 | 0.8845 | 0.0282 | 0.067* | |
C14 | 0.6049 (9) | 0.4565 (7) | 0.3144 (4) | 0.034 (2) | |
H14 | 0.5546 | 0.4239 | 0.2812 | 0.041* | |
C15 | 0.7192 (10) | 0.4050 (8) | 0.3379 (4) | 0.039 (2) | |
H15 | 0.7464 | 0.3399 | 0.3201 | 0.046* | |
C16 | 0.7928 (9) | 0.4468 (9) | 0.3863 (4) | 0.040 (2) | |
C17 | 0.7474 (11) | 0.5455 (8) | 0.4109 (4) | 0.046 (3) | |
H17 | 0.7949 | 0.5781 | 0.4447 | 0.055* | |
C18 | 0.6338 (10) | 0.5924 (8) | 0.3848 (4) | 0.040 (2) | |
H18 | 0.6040 | 0.6578 | 0.4015 | 0.047* | |
C19 | 1.0096 (12) | 0.4825 (12) | 0.3309 (5) | 0.083 (4) | |
H19A | 1.0853 | 0.5294 | 0.3332 | 0.124* | |
H19B | 0.9357 | 0.5328 | 0.3257 | 0.124* | |
H19C | 1.0005 | 0.4293 | 0.2990 | 0.124* | |
C20 | 1.0203 (12) | 0.4164 (11) | 0.3833 (5) | 0.064 (3) | |
C21 | 0.9210 (11) | 0.3978 (8) | 0.4121 (4) | 0.045 (3) | |
C22 | 0.9372 (11) | 0.3346 (11) | 0.4607 (5) | 0.059 (3) | |
C23 | 0.8322 (13) | 0.3104 (16) | 0.4899 (5) | 0.102 (5) | |
H23A | 0.8365 | 0.2298 | 0.5022 | 0.153* | |
H23B | 0.7514 | 0.3245 | 0.4638 | 0.153* | |
H23C | 0.8399 | 0.3609 | 0.5227 | 0.153* | |
Cl1S | 0.2166 (4) | 0.3560 (3) | 0.11919 (15) | 0.0815 (10) | |
Cl2S | −0.0285 (5) | 0.3272 (5) | 0.1385 (2) | 0.1329 (18) | |
Cl3S | 0.0342 (6) | 0.5336 (5) | 0.0859 (3) | 0.170 (2) | |
C1S | 0.0705 (17) | 0.3922 (13) | 0.0883 (6) | 0.113 (7) | |
H1S | 0.0461 | 0.3569 | 0.0499 | 0.135* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.0497 (3) | 0.0274 (2) | 0.0299 (2) | 0.00554 (18) | 0.01803 (16) | 0.00292 (15) |
Cl1 | 0.075 (2) | 0.0287 (12) | 0.0353 (12) | 0.0014 (12) | 0.0183 (12) | 0.0000 (9) |
O1 | 0.051 (5) | 0.039 (4) | 0.057 (4) | −0.001 (4) | 0.016 (4) | 0.002 (3) |
O2 | 0.095 (7) | 0.042 (4) | 0.048 (4) | 0.012 (4) | 0.051 (4) | 0.011 (3) |
O3 | 0.064 (6) | 0.065 (5) | 0.081 (6) | 0.024 (5) | 0.030 (5) | 0.033 (4) |
O4 | 0.073 (6) | 0.039 (4) | 0.038 (3) | −0.001 (3) | 0.030 (4) | −0.005 (3) |
O5 | 0.057 (5) | 0.041 (4) | 0.036 (3) | −0.003 (3) | 0.019 (3) | 0.008 (3) |
O6 | 0.045 (6) | 0.083 (6) | 0.093 (6) | 0.005 (5) | 0.014 (5) | 0.007 (5) |
O7 | 0.066 (7) | 0.088 (7) | 0.064 (5) | 0.012 (5) | 0.007 (5) | 0.008 (4) |
N1 | 0.054 (5) | 0.025 (4) | 0.034 (4) | 0.005 (4) | 0.023 (4) | 0.005 (3) |
N2 | 0.047 (5) | 0.031 (4) | 0.026 (4) | −0.003 (4) | 0.012 (3) | 0.000 (3) |
C1 | 0.046 (7) | 0.054 (7) | 0.036 (5) | 0.022 (5) | 0.021 (5) | 0.018 (5) |
C2 | 0.090 (9) | 0.020 (5) | 0.048 (6) | 0.015 (5) | 0.028 (6) | 0.001 (4) |
C3 | 0.052 (8) | 0.038 (6) | 0.057 (6) | 0.010 (5) | 0.029 (6) | 0.019 (5) |
C4 | 0.055 (7) | 0.029 (5) | 0.030 (5) | −0.006 (4) | 0.019 (5) | −0.004 (4) |
C5 | 0.051 (7) | 0.035 (5) | 0.033 (5) | −0.016 (4) | 0.016 (5) | 0.005 (4) |
C6 | 0.050 (6) | 0.023 (4) | 0.027 (4) | −0.005 (4) | 0.012 (4) | −0.002 (3) |
C7 | 0.052 (7) | 0.028 (5) | 0.025 (4) | 0.004 (4) | 0.007 (4) | −0.001 (3) |
C8 | 0.036 (6) | 0.037 (5) | 0.029 (4) | −0.004 (4) | 0.009 (4) | −0.003 (4) |
C9 | 0.071 (8) | 0.039 (5) | 0.043 (6) | 0.009 (5) | 0.029 (5) | −0.004 (4) |
C10 | 0.055 (7) | 0.039 (5) | 0.030 (5) | −0.003 (5) | 0.017 (5) | −0.003 (4) |
C11 | 0.046 (6) | 0.027 (5) | 0.028 (4) | −0.002 (4) | 0.013 (4) | −0.002 (3) |
C12 | 0.037 (6) | 0.035 (5) | 0.031 (5) | −0.004 (4) | 0.008 (4) | 0.002 (4) |
C13 | 0.057 (7) | 0.031 (5) | 0.048 (6) | −0.001 (5) | 0.015 (5) | −0.002 (4) |
C14 | 0.040 (6) | 0.028 (5) | 0.035 (5) | 0.000 (4) | 0.009 (4) | −0.010 (4) |
C15 | 0.044 (7) | 0.041 (5) | 0.032 (5) | 0.000 (4) | 0.012 (4) | −0.010 (4) |
C16 | 0.030 (6) | 0.056 (6) | 0.035 (5) | 0.006 (5) | 0.008 (4) | 0.007 (4) |
C17 | 0.068 (8) | 0.038 (6) | 0.034 (5) | −0.006 (5) | 0.014 (5) | −0.010 (4) |
C18 | 0.055 (7) | 0.033 (5) | 0.033 (5) | 0.005 (5) | 0.015 (5) | −0.002 (4) |
C19 | 0.052 (9) | 0.122 (12) | 0.080 (9) | −0.011 (8) | 0.025 (7) | 0.028 (8) |
C20 | 0.049 (9) | 0.061 (7) | 0.076 (8) | −0.006 (6) | 0.001 (7) | −0.004 (6) |
C21 | 0.054 (7) | 0.044 (6) | 0.041 (6) | 0.003 (5) | 0.016 (5) | −0.005 (4) |
C22 | 0.042 (8) | 0.082 (8) | 0.050 (7) | 0.017 (6) | 0.006 (5) | 0.010 (6) |
C23 | 0.060 (10) | 0.192 (16) | 0.060 (8) | 0.003 (10) | 0.026 (7) | 0.049 (10) |
Cl1S | 0.096 (3) | 0.073 (2) | 0.078 (2) | −0.0042 (19) | 0.027 (2) | −0.0085 (17) |
Cl2S | 0.102 (4) | 0.188 (5) | 0.118 (4) | −0.034 (4) | 0.044 (3) | 0.011 (4) |
Cl3S | 0.131 (5) | 0.118 (4) | 0.236 (7) | 0.015 (4) | −0.018 (5) | 0.037 (4) |
C1S | 0.120 (15) | 0.099 (12) | 0.084 (10) | 0.041 (10) | −0.053 (10) | −0.032 (9) |
Re1—Cl1 | 2.465 (2) | C9—H9C | 0.9800 |
Re1—N1 | 2.237 (7) | C10—C11 | 1.412 (12) |
Re1—N2 | 2.202 (8) | C11—C12 | 1.402 (11) |
Re1—C1 | 1.954 (12) | C12—C13 | 1.489 (12) |
Re1—C2 | 1.901 (10) | C13—H13A | 0.9800 |
Re1—C3 | 1.915 (12) | C13—H13B | 0.9800 |
O1—C1 | 1.117 (12) | C13—H13C | 0.9800 |
O2—C2 | 1.174 (11) | C14—C15 | 1.388 (13) |
O3—C3 | 1.151 (12) | C14—H14 | 0.9500 |
C10—O4 | 1.302 (10) | C15—C16 | 1.362 (13) |
C12—O5 | 1.301 (10) | C15—H15 | 0.9500 |
O5—H5O | 1.13 (11) | C16—C17 | 1.428 (13) |
C20—O6 | 1.309 (14) | C16—C21 | 1.512 (14) |
C22—O7 | 1.290 (13) | C17—C18 | 1.375 (14) |
O7—H7O | 1.06 (15) | C17—H17 | 0.9500 |
N1—C4 | 1.315 (12) | C18—H18 | 0.9500 |
N1—C8 | 1.355 (11) | C19—C20 | 1.470 (16) |
N2—C14 | 1.340 (10) | C19—H19A | 0.9800 |
N2—C18 | 1.349 (11) | C19—H19B | 0.9800 |
C4—C5 | 1.398 (12) | C19—H19C | 0.9800 |
C4—H4 | 0.9500 | C20—C21 | 1.426 (15) |
C5—C6 | 1.375 (12) | C21—C22 | 1.369 (14) |
C5—H5 | 0.9500 | C22—C23 | 1.496 (16) |
C6—C7 | 1.388 (13) | C23—H23A | 0.9800 |
C6—C11 | 1.511 (11) | C23—H23B | 0.9800 |
C7—C8 | 1.385 (11) | C23—H23C | 0.9800 |
C7—H7 | 0.9500 | Cl1S—C1S | 1.660 (16) |
C8—H8 | 0.9500 | Cl2S—C1S | 1.95 (2) |
C9—C10 | 1.498 (12) | Cl3S—C1S | 1.687 (14) |
C9—H9A | 0.9800 | C1S—H1S | 1.0000 |
C9—H9B | 0.9800 | ||
Cl1—Re1—N2 | 86.08 (19) | C12—C11—C6 | 120.6 (7) |
Cl1—Re1—N1 | 84.81 (19) | C10—C11—C6 | 119.6 (7) |
C2—Re1—C3 | 87.1 (4) | O5—C12—C11 | 120.6 (8) |
C2—Re1—C1 | 90.6 (4) | O5—C12—C13 | 116.0 (8) |
C3—Re1—C1 | 87.9 (4) | C11—C12—C13 | 123.4 (8) |
C2—Re1—N2 | 91.8 (4) | C12—C13—H13A | 109.5 |
C3—Re1—N2 | 178.9 (3) | C12—C13—H13B | 109.5 |
C1—Re1—N2 | 92.4 (3) | H13A—C13—H13B | 109.5 |
C2—Re1—N1 | 175.2 (4) | C12—C13—H13C | 109.5 |
C3—Re1—N1 | 96.9 (3) | H13A—C13—H13C | 109.5 |
C1—Re1—N1 | 92.2 (3) | H13B—C13—H13C | 109.5 |
N1—Re1—N2 | 84.1 (3) | N2—C14—C15 | 122.7 (8) |
C2—Re1—Cl1 | 92.3 (3) | N2—C14—H14 | 118.7 |
C3—Re1—Cl1 | 93.7 (3) | C15—C14—H14 | 118.7 |
C1—Re1—Cl1 | 176.8 (3) | C16—C15—C14 | 120.7 (8) |
C10—O4—H5O | 104 (4) | C16—C15—H15 | 119.6 |
C12—O5—H5O | 109 (5) | C14—C15—H15 | 119.6 |
C20—O6—H7O | 98 (6) | C15—C16—C17 | 117.0 (9) |
C22—O7—H7O | 99 (8) | C15—C16—C21 | 122.9 (9) |
C4—N1—C8 | 118.4 (7) | C17—C16—C21 | 120.0 (9) |
C4—N1—Re1 | 122.0 (6) | C18—C17—C16 | 118.9 (9) |
C8—N1—Re1 | 119.5 (6) | C18—C17—H17 | 120.6 |
C14—N2—C18 | 117.4 (8) | C16—C17—H17 | 120.6 |
C14—N2—Re1 | 121.3 (6) | N2—C18—C17 | 123.2 (8) |
C18—N2—Re1 | 121.2 (6) | N2—C18—H18 | 118.4 |
O1—C1—Re1 | 179.3 (10) | C17—C18—H18 | 118.4 |
O2—C2—Re1 | 177.2 (11) | C20—C19—H19A | 109.5 |
O3—C3—Re1 | 177.8 (10) | C20—C19—H19B | 109.5 |
N1—C4—C5 | 122.8 (9) | H19A—C19—H19B | 109.5 |
N1—C4—H4 | 118.6 | C20—C19—H19C | 109.5 |
C5—C4—H4 | 118.6 | H19A—C19—H19C | 109.5 |
C6—C5—C4 | 119.6 (9) | H19B—C19—H19C | 109.5 |
C6—C5—H5 | 120.2 | O6—C20—C21 | 117.3 (11) |
C4—C5—H5 | 120.2 | O6—C20—C19 | 117.4 (12) |
C5—C6—C7 | 117.4 (8) | C21—C20—C19 | 125.3 (11) |
C5—C6—C11 | 120.5 (9) | C22—C21—C20 | 122.3 (11) |
C7—C6—C11 | 122.0 (8) | C22—C21—C16 | 119.6 (9) |
C8—C7—C6 | 120.2 (8) | C20—C21—C16 | 118.0 (9) |
C8—C7—H7 | 119.9 | O7—C22—C21 | 122.1 (11) |
C6—C7—H7 | 119.9 | O7—C22—C23 | 115.2 (11) |
N1—C8—C7 | 121.5 (9) | C21—C22—C23 | 122.7 (11) |
N1—C8—H8 | 119.2 | C22—C23—H23A | 109.5 |
C7—C8—H8 | 119.2 | C22—C23—H23B | 109.5 |
C10—C9—H9A | 109.5 | H23A—C23—H23B | 109.5 |
C10—C9—H9B | 109.5 | C22—C23—H23C | 109.5 |
H9A—C9—H9B | 109.5 | H23A—C23—H23C | 109.5 |
C10—C9—H9C | 109.5 | H23B—C23—H23C | 109.5 |
H9A—C9—H9C | 109.5 | Cl1S—C1S—Cl3S | 117.2 (10) |
H9B—C9—H9C | 109.5 | Cl1S—C1S—Cl2S | 102.9 (8) |
O4—C10—C11 | 120.7 (8) | Cl3S—C1S—Cl2S | 103.9 (9) |
O4—C10—C9 | 116.2 (8) | Cl1S—C1S—H1S | 110.7 |
C11—C10—C9 | 123.1 (8) | Cl3S—C1S—H1S | 110.7 |
C12—C11—C10 | 119.8 (8) | Cl2S—C1S—H1S | 110.7 |
C3—Re1—N1—C4 | 132.5 (7) | C5—C6—C11—C12 | −76.2 (12) |
C1—Re1—N1—C4 | −139.4 (7) | C7—C6—C11—C12 | 99.4 (11) |
N2—Re1—N1—C4 | −47.2 (7) | C5—C6—C11—C10 | 102.1 (11) |
Cl1—Re1—N1—C4 | 39.4 (7) | C7—C6—C11—C10 | −82.3 (12) |
C3—Re1—N1—C8 | −43.5 (7) | C10—C11—C12—O5 | −1.0 (15) |
C1—Re1—N1—C8 | 44.6 (7) | C6—C11—C12—O5 | 177.3 (9) |
N2—Re1—N1—C8 | 136.8 (6) | C10—C11—C12—C13 | 176.5 (9) |
Cl1—Re1—N1—C8 | −136.6 (6) | C6—C11—C12—C13 | −5.2 (15) |
C2—Re1—N2—C14 | 129.4 (7) | C18—N2—C14—C15 | −2.1 (13) |
C1—Re1—N2—C14 | 38.7 (7) | Re1—N2—C14—C15 | 180.0 (7) |
N1—Re1—N2—C14 | −53.3 (6) | N2—C14—C15—C16 | 1.8 (14) |
Cl1—Re1—N2—C14 | −138.4 (6) | C14—C15—C16—C17 | −0.6 (14) |
C2—Re1—N2—C18 | −48.4 (7) | C14—C15—C16—C21 | −176.8 (9) |
C1—Re1—N2—C18 | −139.0 (7) | C15—C16—C17—C18 | −0.1 (14) |
N1—Re1—N2—C18 | 129.0 (7) | C21—C16—C17—C18 | 176.3 (9) |
Cl1—Re1—N2—C18 | 43.8 (6) | C14—N2—C18—C17 | 1.4 (13) |
C8—N1—C4—C5 | −2.8 (13) | Re1—N2—C18—C17 | 179.3 (7) |
Re1—N1—C4—C5 | −178.9 (6) | C16—C17—C18—N2 | −0.3 (14) |
N1—C4—C5—C6 | 0.7 (14) | O6—C20—C21—C22 | 0.0 (17) |
C4—C5—C6—C7 | 2.0 (13) | C19—C20—C21—C22 | 179.6 (12) |
C4—C5—C6—C11 | 177.8 (8) | O6—C20—C21—C16 | −177.9 (10) |
C5—C6—C7—C8 | −2.5 (13) | C19—C20—C21—C16 | 1.8 (17) |
C11—C6—C7—C8 | −178.3 (7) | C15—C16—C21—C22 | −108.2 (12) |
C4—N1—C8—C7 | 2.3 (12) | C17—C16—C21—C22 | 75.6 (13) |
Re1—N1—C8—C7 | 178.4 (6) | C15—C16—C21—C20 | 69.7 (14) |
C6—C7—C8—N1 | 0.4 (13) | C17—C16—C21—C20 | −106.5 (11) |
O4—C10—C11—C12 | 1.4 (15) | C20—C21—C22—O7 | 0.3 (19) |
C9—C10—C11—C12 | −179.0 (10) | C16—C21—C22—O7 | 178.1 (10) |
O4—C10—C11—C6 | −176.9 (9) | C20—C21—C22—C23 | −177.3 (13) |
C9—C10—C11—C6 | 2.7 (15) | C16—C21—C22—C23 | 0.5 (19) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5O···O4 | 1.13 (11) | 1.46 (11) | 2.459 (9) | 144 (8) |
O7—H7O···O6 | 1.06 (15) | 1.55 (14) | 2.486 (12) | 144 (13) |
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