Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807008070/kj2047sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807008070/kj2047Isup2.hkl |
CCDC reference: 640401
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.006 Å
- R factor = 0.035
- wR factor = 0.094
- Data-to-parameter ratio = 15.2
checkCIF/PLATON results
No syntax errors found
Alert level A ABSTM02_ALERT_3_A Crystal and compound unsuitable for non-numerical corrections. Product of mu and tmid > 3.0 Value of mu given = 8.986 tmid = 0.350
Author Response: ... |
See next PLAT065_ALERT_3_A Crystal Requires Numerical Correction mu*tmid .. 3.15
Author Response: ... |
The crystalline fragment used was irregular and its faces were poorly defined, making it difficult to apply an absorption correction based on crystal morphology. The correction with SADABS was assumed to be satisfactory, considering that the R factors was very low, the thermal ellipsoids were normal and no unreasonable discrepancy was noted between this structure and that of the non-N-methyl derivative described in the previous paper.
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Re1 - O1 .. 5.01 su
2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1999); cell refinement: SMART; data reduction: SAINT (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: UdMX (Maris, 2004).
(C24H20P)[Re(C11H11N3O3S)O] | F(000) = 1568 |
Mr = 790.86 | Dx = 1.670 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: -P 2ybc | Cell parameters from 5687 reflections |
a = 13.7077 (2) Å | θ = 3.5–72.6° |
b = 12.5262 (2) Å | µ = 8.99 mm−1 |
c = 19.4526 (3) Å | T = 100 K |
β = 109.700 (1)° | Block, red |
V = 3144.62 (8) Å3 | 0.50 × 0.35 × 0.22 mm |
Z = 4 |
Bruker SMART 2K/PLATFORM diffractometer | 6047 independent reflections |
Radiation source: sealed tube | 5633 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
Detector resolution: 5.5 pixels mm-1 | θmax = 72.9°, θmin = 3.4° |
ω scans | h = −16→16 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −15→15 |
Tmin = 0.057, Tmax = 0.138 | l = −24→23 |
20287 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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.094 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0674P)2 + 1.2591P] where P = (Fo2 + 2Fc2)/3 |
6047 reflections | (Δ/σ)max = 0.002 |
398 parameters | Δρmax = 1.67 e Å−3 |
0 restraints | Δρmin = −1.88 e Å−3 |
Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis. |
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 | 0.281001 (12) | 0.781800 (11) | 0.108341 (8) | 0.01429 (8) | |
O1 | 0.2347 (2) | 0.7944 (2) | 0.01574 (15) | 0.0215 (6) | |
N1 | 0.1691 (3) | 0.8145 (3) | 0.14859 (19) | 0.0233 (7) | |
C1 | 0.1380 (4) | 0.9186 (3) | 0.1668 (3) | 0.0337 (10) | |
H1A | 0.0717 | 0.9389 | 0.1303 | 0.051* | |
H1B | 0.1908 | 0.9715 | 0.1672 | 0.051* | |
H1C | 0.1305 | 0.9156 | 0.2151 | 0.051* | |
C2 | 0.1092 (3) | 0.7270 (3) | 0.1555 (2) | 0.0181 (8) | |
C3 | 0.1514 (3) | 0.6258 (3) | 0.14904 (19) | 0.0167 (7) | |
N4 | 0.2488 (2) | 0.6366 (2) | 0.13925 (15) | 0.0122 (6) | |
C5 | 0.3214 (3) | 0.5574 (3) | 0.15464 (18) | 0.0151 (7) | |
O5 | 0.3107 (2) | 0.4652 (2) | 0.17139 (13) | 0.0191 (5) | |
C6 | 0.4242 (3) | 0.5973 (3) | 0.15014 (19) | 0.0171 (7) | |
H6A | 0.4817 | 0.5754 | 0.1944 | 0.020* | |
H6B | 0.4363 | 0.5659 | 0.1070 | 0.020* | |
N7 | 0.4207 (2) | 0.7143 (2) | 0.14424 (18) | 0.0156 (6) | |
C8 | 0.5131 (3) | 0.7663 (3) | 0.1675 (2) | 0.0176 (7) | |
O8 | 0.5978 (2) | 0.7207 (2) | 0.18738 (16) | 0.0218 (6) | |
C9 | 0.5049 (3) | 0.8865 (3) | 0.1662 (2) | 0.0238 (8) | |
H9A | 0.5229 | 0.9145 | 0.1244 | 0.029* | |
H9B | 0.5554 | 0.9158 | 0.2115 | 0.029* | |
S10 | 0.37452 (7) | 0.93203 (7) | 0.15832 (5) | 0.0211 (2) | |
C21 | 0.0134 (3) | 0.7312 (3) | 0.1673 (2) | 0.0235 (8) | |
H21 | −0.0155 | 0.7980 | 0.1735 | 0.028* | |
C22 | −0.0382 (3) | 0.6377 (4) | 0.1699 (2) | 0.0259 (9) | |
H22 | −0.1030 | 0.6408 | 0.1776 | 0.031* | |
C23 | 0.0026 (3) | 0.5390 (3) | 0.16139 (19) | 0.0217 (8) | |
H23 | −0.0348 | 0.4756 | 0.1626 | 0.026* | |
C24 | 0.0984 (3) | 0.5329 (3) | 0.15101 (18) | 0.0194 (8) | |
H24 | 0.1267 | 0.4656 | 0.1454 | 0.023* | |
P1 | 0.28918 (7) | 0.24112 (7) | 0.02288 (5) | 0.01294 (18) | |
C31 | 0.4222 (3) | 0.2143 (3) | 0.0759 (2) | 0.0139 (7) | |
C32 | 0.4769 (3) | 0.1345 (3) | 0.0556 (2) | 0.0189 (7) | |
H32 | 0.4427 | 0.0889 | 0.0157 | 0.023* | |
C33 | 0.5816 (3) | 0.1211 (3) | 0.0936 (2) | 0.0224 (8) | |
H33 | 0.6197 | 0.0678 | 0.0789 | 0.027* | |
C34 | 0.6309 (3) | 0.1860 (3) | 0.1534 (2) | 0.0218 (8) | |
H34 | 0.7021 | 0.1751 | 0.1804 | 0.026* | |
C35 | 0.5765 (3) | 0.2666 (3) | 0.1737 (2) | 0.0196 (8) | |
H35 | 0.6107 | 0.3114 | 0.2140 | 0.023* | |
C36 | 0.4717 (3) | 0.2815 (3) | 0.1347 (2) | 0.0170 (8) | |
H36 | 0.4341 | 0.3369 | 0.1479 | 0.020* | |
C41 | 0.2868 (3) | 0.3744 (3) | −0.01149 (18) | 0.0155 (7) | |
C42 | 0.3605 (3) | 0.4038 (3) | −0.0436 (2) | 0.0219 (8) | |
H42 | 0.4105 | 0.3535 | −0.0470 | 0.026* | |
C43 | 0.3598 (3) | 0.5065 (3) | −0.0700 (2) | 0.0284 (9) | |
H43 | 0.4084 | 0.5259 | −0.0930 | 0.034* | |
C44 | 0.2891 (3) | 0.5808 (3) | −0.0634 (2) | 0.0246 (8) | |
H44 | 0.2899 | 0.6514 | −0.0811 | 0.030* | |
C45 | 0.2171 (3) | 0.5524 (3) | −0.03104 (19) | 0.0198 (8) | |
H45 | 0.1688 | 0.6037 | −0.0262 | 0.024* | |
C46 | 0.2154 (3) | 0.4489 (3) | −0.00564 (18) | 0.0171 (7) | |
H46 | 0.1651 | 0.4292 | 0.0158 | 0.020* | |
C51 | 0.2043 (3) | 0.2313 (3) | 0.0755 (2) | 0.0154 (7) | |
C52 | 0.2434 (3) | 0.2120 (3) | 0.1505 (2) | 0.0168 (8) | |
H52 | 0.3158 | 0.2042 | 0.1750 | 0.020* | |
C53 | 0.1729 (3) | 0.2043 (3) | 0.1891 (2) | 0.0184 (8) | |
H53 | 0.1979 | 0.1909 | 0.2402 | 0.022* | |
C54 | 0.0677 (3) | 0.2164 (3) | 0.1530 (2) | 0.0214 (8) | |
H54 | 0.0211 | 0.2127 | 0.1796 | 0.026* | |
C55 | 0.0292 (3) | 0.2340 (3) | 0.0775 (2) | 0.0199 (8) | |
H55 | −0.0432 | 0.2410 | 0.0528 | 0.024* | |
C56 | 0.0983 (3) | 0.2410 (3) | 0.0390 (2) | 0.0180 (7) | |
H56 | 0.0729 | 0.2526 | −0.0123 | 0.022* | |
C61 | 0.2434 (3) | 0.1461 (3) | −0.05036 (17) | 0.0131 (6) | |
C62 | 0.1976 (3) | 0.0523 (3) | −0.0373 (2) | 0.0189 (7) | |
H62 | 0.1927 | 0.0387 | 0.0094 | 0.023* | |
C63 | 0.1595 (3) | −0.0207 (3) | −0.0936 (2) | 0.0200 (7) | |
H63 | 0.1276 | −0.0845 | −0.0853 | 0.024* | |
C64 | 0.1675 (3) | −0.0019 (3) | −0.16173 (19) | 0.0189 (7) | |
H64 | 0.1396 | −0.0517 | −0.2002 | 0.023* | |
C65 | 0.2161 (3) | 0.0898 (3) | −0.17368 (19) | 0.0191 (7) | |
H65 | 0.2237 | 0.1015 | −0.2199 | 0.023* | |
C66 | 0.2538 (3) | 0.1644 (3) | −0.11836 (19) | 0.0164 (7) | |
H66 | 0.2864 | 0.2276 | −0.1267 | 0.020* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.01831 (12) | 0.01106 (11) | 0.01370 (11) | 0.00128 (5) | 0.00566 (8) | 0.00142 (5) |
O1 | 0.0277 (16) | 0.0176 (12) | 0.0210 (14) | 0.0006 (10) | 0.0104 (12) | 0.0034 (10) |
N1 | 0.0261 (18) | 0.0189 (16) | 0.0270 (17) | 0.0022 (14) | 0.0117 (14) | 0.0037 (14) |
C1 | 0.034 (2) | 0.023 (2) | 0.047 (3) | 0.0076 (18) | 0.017 (2) | −0.0086 (19) |
C2 | 0.023 (2) | 0.0206 (18) | 0.0141 (18) | 0.0018 (14) | 0.0108 (16) | −0.0028 (13) |
C3 | 0.0161 (18) | 0.0224 (18) | 0.0117 (15) | 0.0016 (14) | 0.0048 (13) | −0.0011 (13) |
N4 | 0.0145 (15) | 0.0116 (13) | 0.0111 (13) | 0.0015 (10) | 0.0050 (11) | 0.0015 (10) |
C5 | 0.0202 (19) | 0.0142 (16) | 0.0105 (15) | 0.0019 (13) | 0.0045 (13) | 0.0009 (13) |
O5 | 0.0227 (14) | 0.0155 (12) | 0.0203 (12) | 0.0013 (10) | 0.0086 (11) | 0.0024 (10) |
C6 | 0.0180 (18) | 0.0158 (16) | 0.0191 (17) | 0.0019 (13) | 0.0086 (14) | 0.0027 (13) |
N7 | 0.0154 (16) | 0.0153 (15) | 0.0174 (15) | 0.0008 (10) | 0.0072 (13) | 0.0012 (11) |
C8 | 0.023 (2) | 0.0210 (18) | 0.0099 (16) | −0.0033 (14) | 0.0079 (15) | 0.0019 (13) |
O8 | 0.0177 (15) | 0.0285 (15) | 0.0200 (14) | −0.0018 (10) | 0.0075 (12) | 0.0041 (10) |
C9 | 0.029 (2) | 0.0208 (19) | 0.0226 (19) | −0.0039 (15) | 0.0097 (16) | −0.0001 (15) |
S10 | 0.0272 (5) | 0.0142 (4) | 0.0220 (4) | −0.0020 (3) | 0.0085 (4) | −0.0001 (3) |
C21 | 0.021 (2) | 0.033 (2) | 0.0170 (18) | 0.0064 (16) | 0.0080 (16) | −0.0022 (15) |
C22 | 0.019 (2) | 0.048 (3) | 0.0126 (16) | −0.0003 (17) | 0.0087 (15) | 0.0004 (17) |
C23 | 0.0203 (19) | 0.034 (2) | 0.0111 (16) | −0.0048 (16) | 0.0057 (14) | 0.0021 (15) |
C24 | 0.023 (2) | 0.0241 (18) | 0.0111 (16) | −0.0030 (15) | 0.0062 (14) | −0.0003 (14) |
P1 | 0.0167 (4) | 0.0124 (4) | 0.0114 (4) | −0.0006 (3) | 0.0071 (3) | 0.0001 (3) |
C31 | 0.0137 (18) | 0.0182 (18) | 0.0113 (16) | −0.0003 (12) | 0.0060 (14) | 0.0041 (12) |
C32 | 0.0223 (19) | 0.0146 (16) | 0.0203 (17) | −0.0008 (14) | 0.0076 (15) | −0.0016 (13) |
C33 | 0.023 (2) | 0.0155 (16) | 0.030 (2) | 0.0034 (14) | 0.0108 (16) | −0.0013 (15) |
C34 | 0.019 (2) | 0.0243 (18) | 0.0226 (19) | 0.0009 (15) | 0.0070 (15) | 0.0020 (16) |
C35 | 0.026 (2) | 0.0187 (17) | 0.0146 (17) | −0.0036 (15) | 0.0085 (16) | −0.0014 (14) |
C36 | 0.022 (2) | 0.0144 (17) | 0.0171 (18) | −0.0026 (13) | 0.0104 (16) | −0.0006 (12) |
C41 | 0.0222 (19) | 0.0138 (16) | 0.0105 (15) | −0.0030 (13) | 0.0057 (14) | −0.0009 (12) |
C42 | 0.028 (2) | 0.0179 (17) | 0.0261 (19) | 0.0027 (15) | 0.0172 (16) | 0.0021 (15) |
C43 | 0.038 (2) | 0.0213 (19) | 0.035 (2) | −0.0015 (17) | 0.0242 (19) | 0.0061 (17) |
C44 | 0.036 (2) | 0.0142 (17) | 0.0249 (19) | 0.0021 (15) | 0.0124 (17) | 0.0025 (15) |
C45 | 0.025 (2) | 0.0154 (17) | 0.0163 (16) | 0.0016 (14) | 0.0035 (14) | −0.0021 (14) |
C46 | 0.0208 (19) | 0.0180 (17) | 0.0132 (15) | −0.0024 (14) | 0.0068 (14) | −0.0015 (13) |
C51 | 0.020 (2) | 0.0128 (15) | 0.0158 (17) | −0.0022 (13) | 0.0099 (15) | −0.0021 (12) |
C52 | 0.021 (2) | 0.0165 (18) | 0.0161 (18) | −0.0024 (13) | 0.0110 (16) | −0.0016 (13) |
C53 | 0.025 (2) | 0.0187 (17) | 0.0151 (17) | −0.0055 (14) | 0.0122 (16) | −0.0008 (13) |
C54 | 0.028 (2) | 0.0173 (19) | 0.027 (2) | −0.0033 (13) | 0.0204 (18) | −0.0027 (14) |
C55 | 0.0164 (19) | 0.0201 (17) | 0.024 (2) | −0.0006 (14) | 0.0075 (16) | 0.0020 (15) |
C56 | 0.024 (2) | 0.0190 (17) | 0.0124 (17) | 0.0005 (15) | 0.0083 (15) | 0.0021 (14) |
C61 | 0.0159 (17) | 0.0130 (16) | 0.0101 (15) | −0.0011 (13) | 0.0039 (13) | −0.0021 (12) |
C62 | 0.024 (2) | 0.0176 (17) | 0.0152 (16) | −0.0016 (14) | 0.0074 (15) | 0.0033 (14) |
C63 | 0.0222 (19) | 0.0154 (17) | 0.0201 (17) | −0.0013 (14) | 0.0041 (15) | 0.0022 (14) |
C64 | 0.022 (2) | 0.0186 (17) | 0.0140 (16) | 0.0054 (14) | 0.0028 (14) | 0.0004 (13) |
C65 | 0.0236 (19) | 0.0209 (17) | 0.0140 (16) | 0.0044 (15) | 0.0080 (14) | −0.0008 (14) |
C66 | 0.0187 (18) | 0.0169 (16) | 0.0168 (16) | 0.0012 (13) | 0.0102 (14) | 0.0011 (13) |
Re1—O1 | 1.703 (3) | C33—C34 | 1.392 (5) |
Re1—N1 | 1.986 (3) | C33—H33 | 0.95 |
Re1—N7 | 1.992 (3) | C34—C35 | 1.389 (6) |
Re1—N4 | 2.011 (3) | C34—H34 | 0.95 |
Re1—S10 | 2.2999 (9) | C35—C36 | 1.393 (6) |
N1—C2 | 1.403 (5) | C35—H35 | 0.95 |
N1—C1 | 1.452 (5) | C36—H36 | 0.95 |
C1—H1a | 0.98 | C41—C46 | 1.384 (5) |
C1—H1b | 0.98 | C41—C42 | 1.404 (5) |
C1—H1c | 0.98 | C42—C43 | 1.385 (5) |
C2—C21 | 1.408 (5) | C42—H42 | 0.95 |
C2—C3 | 1.416 (5) | C43—C44 | 1.381 (6) |
C3—C24 | 1.379 (5) | C43—H43 | 0.95 |
C3—N4 | 1.417 (4) | C44—C45 | 1.385 (6) |
N4—C5 | 1.366 (4) | C44—H44 | 0.95 |
C5—O5 | 1.222 (4) | C45—C46 | 1.390 (5) |
C5—C6 | 1.525 (5) | C45—H45 | 0.95 |
C6—N7 | 1.469 (4) | C46—H46 | 0.95 |
C6—H6a | 0.99 | C51—C56 | 1.390 (6) |
C6—H6b | 0.99 | C51—C52 | 1.395 (5) |
N7—C8 | 1.359 (5) | C52—C53 | 1.414 (5) |
C8—O8 | 1.233 (5) | C52—H52 | 0.95 |
C8—C9 | 1.510 (5) | C53—C54 | 1.382 (6) |
C9—S10 | 1.832 (4) | C53—H53 | 0.95 |
C9—H9a | 0.99 | C54—C55 | 1.401 (6) |
C9—H9b | 0.99 | C54—H54 | 0.95 |
C21—C22 | 1.377 (6) | C55—C56 | 1.394 (5) |
C21—H21 | 0.95 | C55—H55 | 0.95 |
C22—C23 | 1.389 (6) | C56—H56 | 0.95 |
C22—H22 | 0.95 | C61—C62 | 1.394 (5) |
C23—C24 | 1.397 (5) | C61—C66 | 1.396 (5) |
C23—H23 | 0.95 | C62—C63 | 1.387 (5) |
C24—H24 | 0.95 | C62—H62 | 0.95 |
P1—C51 | 1.795 (4) | C63—C64 | 1.387 (5) |
P1—C41 | 1.795 (3) | C63—H63 | 0.95 |
P1—C31 | 1.798 (4) | C64—C65 | 1.386 (5) |
P1—C61 | 1.799 (3) | C64—H64 | 0.95 |
C31—C32 | 1.384 (5) | C65—C66 | 1.387 (5) |
C31—C36 | 1.398 (5) | C65—H65 | 0.95 |
C32—C33 | 1.384 (5) | C66—H66 | 0.95 |
C32—H32 | 0.95 | ||
O1—Re1—N1 | 109.60 (14) | C36—C31—P1 | 118.4 (3) |
O1—Re1—N4 | 111.04 (11) | C31—C32—C33 | 119.9 (3) |
N1—Re1—N4 | 77.98 (13) | C31—C32—H32 | 120.1 |
O1—Re1—N7 | 112.44 (13) | C33—C32—H32 | 120.1 |
N1—Re1—N7 | 136.76 (14) | C32—C33—C34 | 119.9 (4) |
N4—Re1—N7 | 78.09 (11) | C32—C33—H33 | 120 |
O1—Re1—S10 | 109.09 (9) | C34—C33—H33 | 120 |
N1—Re1—S10 | 93.39 (10) | C35—C34—C33 | 120.4 (4) |
N4—Re1—S10 | 139.55 (8) | C35—C34—H34 | 119.8 |
N7—Re1—S10 | 82.30 (8) | C33—C34—H34 | 119.8 |
C2—N1—C1 | 116.7 (3) | C34—C35—C36 | 119.8 (3) |
C2—N1—Re1 | 115.6 (3) | C34—C35—H35 | 120.1 |
C1—N1—Re1 | 127.6 (3) | C36—C35—H35 | 120.1 |
N1—C1—H1A | 109.5 | C35—C36—C31 | 119.4 (3) |
N1—C1—H1B | 109.5 | C35—C36—H36 | 120.3 |
H1A—C1—H1B | 109.5 | C31—C36—H36 | 120.3 |
N1—C1—H1C | 109.5 | C46—C41—C42 | 119.7 (3) |
H1A—C1—H1C | 109.5 | C46—C41—P1 | 121.4 (3) |
H1B—C1—H1C | 109.5 | C42—C41—P1 | 118.9 (3) |
N1—C2—C21 | 126.5 (3) | C43—C42—C41 | 119.5 (4) |
N1—C2—C3 | 114.9 (4) | C43—C42—H42 | 120.2 |
C21—C2—C3 | 118.6 (3) | C41—C42—H42 | 120.2 |
C24—C3—C2 | 121.2 (3) | C44—C43—C42 | 120.6 (4) |
C24—C3—N4 | 127.8 (3) | C44—C43—H43 | 119.7 |
C2—C3—N4 | 111.0 (3) | C42—C43—H43 | 119.7 |
C5—N4—C3 | 123.5 (3) | C43—C44—C45 | 119.9 (3) |
C5—N4—Re1 | 120.4 (2) | C43—C44—H44 | 120 |
C3—N4—Re1 | 116.0 (2) | C45—C44—H44 | 120 |
O5—C5—N4 | 126.9 (3) | C44—C45—C46 | 120.1 (4) |
O5—C5—C6 | 121.4 (3) | C44—C45—H45 | 120 |
N4—C5—C6 | 111.6 (3) | C46—C45—H45 | 120 |
N7—C6—C5 | 109.0 (3) | C41—C46—C45 | 120.1 (3) |
N7—C6—H6A | 109.9 | C41—C46—H46 | 119.9 |
C5—C6—H6A | 109.9 | C45—C46—H46 | 119.9 |
N7—C6—H6B | 109.9 | C56—C51—C52 | 121.1 (4) |
C5—C6—H6B | 109.9 | C56—C51—P1 | 118.0 (3) |
H6A—C6—H6B | 108.3 | C52—C51—P1 | 120.9 (3) |
C8—N7—C6 | 116.8 (3) | C51—C52—C53 | 118.5 (4) |
C8—N7—Re1 | 126.2 (2) | C51—C52—H52 | 120.8 |
C6—N7—Re1 | 116.9 (2) | C53—C52—H52 | 120.8 |
O8—C8—N7 | 123.8 (3) | C54—C53—C52 | 120.3 (4) |
O8—C8—C9 | 121.6 (3) | C54—C53—H53 | 119.8 |
N7—C8—C9 | 114.6 (3) | C52—C53—H53 | 119.8 |
C8—C9—S10 | 112.2 (3) | C53—C54—C55 | 120.7 (4) |
C8—C9—H9A | 109.2 | C53—C54—H54 | 119.7 |
S10—C9—H9A | 109.2 | C55—C54—H54 | 119.7 |
C8—C9—H9B | 109.2 | C56—C55—C54 | 119.3 (4) |
S10—C9—H9B | 109.2 | C56—C55—H55 | 120.4 |
H9A—C9—H9B | 107.9 | C54—C55—H55 | 120.4 |
C9—S10—Re1 | 99.76 (12) | C51—C56—C55 | 120.1 (3) |
C22—C21—C2 | 119.5 (4) | C51—C56—H56 | 119.9 |
C22—C21—H21 | 120.3 | C55—C56—H56 | 119.9 |
C2—C21—H21 | 120.3 | C62—C61—C66 | 120.4 (3) |
C21—C22—C23 | 121.4 (4) | C62—C61—P1 | 118.1 (3) |
C21—C22—H22 | 119.3 | C66—C61—P1 | 121.5 (3) |
C23—C22—H22 | 119.3 | C63—C62—C61 | 119.0 (3) |
C22—C23—C24 | 120.1 (4) | C63—C62—H62 | 120.5 |
C22—C23—H23 | 119.9 | C61—C62—H62 | 120.5 |
C24—C23—H23 | 119.9 | C62—C63—C64 | 120.8 (3) |
C3—C24—C23 | 119.2 (4) | C62—C63—H63 | 119.6 |
C3—C24—H24 | 120.4 | C64—C63—H63 | 119.6 |
C23—C24—H24 | 120.4 | C65—C64—C63 | 119.9 (3) |
C51—P1—C41 | 110.02 (17) | C65—C64—H64 | 120 |
C51—P1—C31 | 112.81 (17) | C63—C64—H64 | 120 |
C41—P1—C31 | 105.96 (16) | C64—C65—C66 | 120.1 (3) |
C51—P1—C61 | 106.59 (16) | C64—C65—H65 | 119.9 |
C41—P1—C61 | 111.27 (15) | C66—C65—H65 | 119.9 |
C31—P1—C61 | 110.26 (16) | C65—C66—C61 | 119.6 (3) |
C32—C31—C36 | 120.5 (4) | C65—C66—H66 | 120.2 |
C32—C31—P1 | 120.9 (3) | C61—C66—H66 | 120.2 |
O1—Re1—N1—C2 | 90.5 (3) | C2—C3—C24—C23 | −1.6 (5) |
N7—Re1—N1—C2 | −75.5 (3) | N4—C3—C24—C23 | 179.9 (3) |
N4—Re1—N1—C2 | −17.8 (3) | C22—C23—C24—C3 | −0.3 (5) |
S10—Re1—N1—C2 | −157.8 (3) | C51—P1—C31—C32 | 123.0 (3) |
O1—Re1—N1—C1 | −84.9 (4) | C41—P1—C31—C32 | −116.5 (3) |
N7—Re1—N1—C1 | 109.1 (4) | C61—P1—C31—C32 | 4.0 (3) |
N4—Re1—N1—C1 | 166.8 (4) | C51—P1—C31—C36 | −62.0 (3) |
S10—Re1—N1—C1 | 26.7 (4) | C41—P1—C31—C36 | 58.4 (3) |
C1—N1—C2—C21 | 10.5 (6) | C61—P1—C31—C36 | 178.9 (3) |
Re1—N1—C2—C21 | −165.5 (3) | C36—C31—C32—C33 | −0.3 (5) |
C1—N1—C2—C3 | −170.1 (4) | P1—C31—C32—C33 | 174.6 (3) |
Re1—N1—C2—C3 | 13.9 (4) | C31—C32—C33—C34 | 1.8 (6) |
N1—C2—C3—C24 | −176.7 (3) | C32—C33—C34—C35 | −2.2 (6) |
C21—C2—C3—C24 | 2.8 (6) | C33—C34—C35—C36 | 1.0 (6) |
N1—C2—C3—N4 | 2.1 (5) | C34—C35—C36—C31 | 0.6 (6) |
C21—C2—C3—N4 | −178.5 (3) | C32—C31—C36—C35 | −1.0 (5) |
C24—C3—N4—C5 | −23.3 (5) | P1—C31—C36—C35 | −175.9 (3) |
C2—C3—N4—C5 | 158.1 (3) | C51—P1—C41—C46 | −9.3 (3) |
C24—C3—N4—Re1 | 161.5 (3) | C31—P1—C41—C46 | −131.5 (3) |
C2—C3—N4—Re1 | −17.1 (4) | C61—P1—C41—C46 | 108.6 (3) |
O1—Re1—N4—C5 | 97.3 (3) | C51—P1—C41—C42 | 169.4 (3) |
N1—Re1—N4—C5 | −156.1 (3) | C31—P1—C41—C42 | 47.2 (3) |
N7—Re1—N4—C5 | −12.4 (2) | C61—P1—C41—C42 | −72.7 (3) |
S10—Re1—N4—C5 | −75.1 (3) | C46—C41—C42—C43 | −1.1 (6) |
O1—Re1—N4—C3 | −87.3 (2) | P1—C41—C42—C43 | −179.8 (3) |
N1—Re1—N4—C3 | 19.3 (2) | C41—C42—C43—C44 | 1.7 (6) |
N7—Re1—N4—C3 | 163.0 (3) | C42—C43—C44—C45 | −1.0 (6) |
S10—Re1—N4—C3 | 100.2 (2) | C43—C44—C45—C46 | −0.5 (6) |
C3—N4—C5—O5 | 7.8 (5) | C42—C41—C46—C45 | −0.3 (5) |
Re1—N4—C5—O5 | −177.2 (3) | P1—C41—C46—C45 | 178.3 (3) |
C3—N4—C5—C6 | −171.1 (3) | C44—C45—C46—C41 | 1.1 (5) |
Re1—N4—C5—C6 | 3.9 (4) | C41—P1—C51—C56 | 67.5 (3) |
O5—C5—C6—N7 | −168.2 (3) | C31—P1—C51—C56 | −174.5 (3) |
N4—C5—C6—N7 | 10.7 (4) | C61—P1—C51—C56 | −53.3 (3) |
C5—C6—N7—C8 | 155.3 (3) | C41—P1—C51—C52 | −113.9 (3) |
C5—C6—N7—Re1 | −21.3 (4) | C31—P1—C51—C52 | 4.2 (3) |
O1—Re1—N7—C8 | 94.3 (3) | C61—P1—C51—C52 | 125.3 (3) |
N1—Re1—N7—C8 | −100.0 (3) | C56—C51—C52—C53 | −1.0 (5) |
N4—Re1—N7—C8 | −157.7 (3) | P1—C51—C52—C53 | −179.6 (2) |
S10—Re1—N7—C8 | −13.3 (3) | C51—C52—C53—C54 | −0.4 (5) |
O1—Re1—N7—C6 | −89.5 (3) | C52—C53—C54—C55 | 1.4 (5) |
N1—Re1—N7—C6 | 76.2 (3) | C53—C54—C55—C56 | −1.1 (5) |
N4—Re1—N7—C6 | 18.5 (3) | C52—C51—C56—C55 | 1.4 (5) |
S10—Re1—N7—C6 | 162.9 (3) | P1—C51—C56—C55 | 180.0 (3) |
C6—N7—C8—O8 | 5.8 (5) | C54—C55—C56—C51 | −0.3 (5) |
Re1—N7—C8—O8 | −177.9 (3) | C51—P1—C61—C62 | −32.3 (3) |
C6—N7—C8—C9 | −175.1 (3) | C41—P1—C61—C62 | −152.3 (3) |
Re1—N7—C8—C9 | 1.1 (5) | C31—P1—C61—C62 | 90.4 (3) |
O8—C8—C9—S10 | −164.8 (3) | C51—P1—C61—C66 | 148.3 (3) |
N7—C8—C9—S10 | 16.1 (4) | C41—P1—C61—C66 | 28.3 (3) |
C8—C9—S10—Re1 | −22.2 (3) | C31—P1—C61—C66 | −88.9 (3) |
O1—Re1—S10—C9 | −94.14 (16) | C66—C61—C62—C63 | −2.2 (5) |
N1—Re1—S10—C9 | 153.76 (16) | P1—C61—C62—C63 | 178.4 (3) |
N7—Re1—S10—C9 | 17.01 (16) | C61—C62—C63—C64 | 0.7 (6) |
N4—Re1—S10—C9 | 78.36 (18) | C62—C63—C64—C65 | 1.5 (6) |
N1—C2—C21—C22 | 177.3 (4) | C63—C64—C65—C66 | −2.2 (5) |
C3—C2—C21—C22 | −2.1 (6) | C64—C65—C66—C61 | 0.7 (5) |
C2—C21—C22—C23 | 0.3 (6) | C62—C61—C66—C65 | 1.5 (5) |
C21—C22—C23—C24 | 0.9 (6) | P1—C61—C66—C65 | −179.1 (3) |
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