Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807001894/bi2137sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807001894/bi2137Isup2.hkl |
CCDC reference: 636850
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; 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: SHELXTL.
[Cu2Mo(C4N2S2)3(C24H21NP2)2(C2H3N)2]·2C2H3N | Z = 2 |
Mr = 1572.44 | F(000) = 1592 |
Triclinic, P1 | Dx = 1.404 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.6197 (6) Å | Cell parameters from 8192 reflections |
b = 12.8711 (6) Å | θ = 0.9–25.1° |
c = 23.497 (1) Å | µ = 1.04 mm−1 |
α = 82.079 (1)° | T = 293 K |
β = 79.725 (1)° | Prism, brown |
γ = 88.113 (1)° | 0.50 × 0.45 × 0.40 mm |
V = 3719.4 (3) Å3 |
Siemens SMART CCD diffractometer | 13031 independent reflections |
Radiation source: fine-focus sealed tube | 9643 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
φ and ω scans | θmax = 25.1°, θmin = 0.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→14 |
Tmin = 0.516, Tmax = 0.661 | k = −13→15 |
19485 measured reflections | l = −22→27 |
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)] = 0.062 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 1.23 | w = 1/[σ2(Fo2) + (0.01P)2 + 10.4674P] where P = (Fo2 + 2Fc2)/3 |
13031 reflections | (Δ/σ)max = 0.001 |
838 parameters | Δρmax = 0.51 e Å−3 |
0 restraints | Δρmin = −0.47 e Å−3 |
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 | ||
Mo | 0.89170 (4) | 0.51877 (4) | 0.22809 (2) | 0.04302 (14) | |
Cu1 | 0.54099 (5) | 0.10330 (6) | 0.45144 (3) | 0.04626 (19) | |
Cu2 | 0.55398 (6) | 0.93312 (6) | 0.05877 (3) | 0.04705 (19) | |
P1 | 0.38543 (12) | 0.17367 (11) | 0.49391 (7) | 0.0425 (3) | |
P2 | 0.70136 (12) | 0.04177 (12) | 0.47354 (7) | 0.0441 (4) | |
P3 | 0.50238 (12) | 0.80110 (11) | 0.01520 (7) | 0.0424 (3) | |
P4 | 0.46717 (11) | 1.06596 (11) | 0.10117 (6) | 0.0405 (3) | |
S1 | 0.90430 (13) | 0.42063 (14) | 0.14851 (7) | 0.0578 (4) | |
S2 | 1.08140 (12) | 0.48183 (12) | 0.21509 (7) | 0.0536 (4) | |
S3 | 0.90640 (14) | 0.51988 (13) | 0.32714 (7) | 0.0583 (4) | |
S4 | 0.75863 (14) | 0.39114 (13) | 0.26954 (7) | 0.0575 (4) | |
S5 | 0.95090 (12) | 0.69725 (12) | 0.21167 (8) | 0.0598 (5) | |
S6 | 0.73616 (12) | 0.60034 (12) | 0.19551 (7) | 0.0509 (4) | |
N1 | 1.3141 (5) | 0.3625 (5) | 0.1276 (3) | 0.093 (2) | |
N2 | 1.0692 (5) | 0.2615 (6) | 0.0493 (3) | 0.099 (2) | |
N3 | 0.7839 (7) | 0.4259 (6) | 0.4803 (3) | 0.105 (3) | |
N4 | 0.6029 (4) | 0.2498 (4) | 0.4007 (2) | 0.0639 (15) | |
N5 | 0.8959 (5) | 0.9697 (5) | 0.1500 (4) | 0.117 (3) | |
N6 | 0.6153 (5) | 0.8437 (4) | 0.1315 (2) | 0.0651 (15) | |
N10 | 0.7144 (4) | −0.0895 (4) | 0.4762 (2) | 0.0561 (14) | |
H10 | 0.7755 | −0.1148 | 0.4614 | 0.067* | |
N11 | 0.5197 (4) | 0.0200 (4) | 0.3869 (2) | 0.0572 (13) | |
N13 | 0.7022 (5) | 0.9738 (4) | 0.0141 (2) | 0.0621 (14) | |
N20 | 0.5435 (4) | 0.8199 (3) | −0.05807 (19) | 0.0447 (11) | |
H20 | 0.5719 | 0.7674 | −0.0744 | 0.054* | |
N40 | 0.0776 (8) | 0.2001 (9) | 0.5352 (8) | 0.238 (9) | |
N50 | 0.3778 (16) | 0.6852 (12) | 0.2606 (7) | 0.260 (9) | |
C1 | 1.0580 (5) | 0.3160 (6) | 0.0840 (3) | 0.070 (2) | |
C2 | 1.0370 (5) | 0.3822 (5) | 0.1287 (3) | 0.0560 (16) | |
C3 | 1.1133 (5) | 0.4111 (5) | 0.1571 (3) | 0.0538 (16) | |
C4 | 1.2247 (6) | 0.3836 (5) | 0.1401 (3) | 0.0668 (19) | |
C5 | 0.6650 (5) | 0.3102 (5) | 0.3768 (3) | 0.0543 (16) | |
C6 | 0.7447 (5) | 0.3821 (4) | 0.3441 (3) | 0.0519 (15) | |
C7 | 0.8077 (5) | 0.4372 (5) | 0.3696 (3) | 0.0535 (16) | |
C8 | 0.7959 (6) | 0.4305 (5) | 0.4306 (3) | 0.069 (2) | |
C9 | 0.6797 (5) | 0.7936 (5) | 0.1519 (3) | 0.0508 (15) | |
C10 | 0.7598 (4) | 0.7318 (4) | 0.1761 (3) | 0.0463 (14) | |
C11 | 0.8536 (5) | 0.7747 (5) | 0.1825 (3) | 0.0534 (16) | |
C12 | 0.8766 (5) | 0.8833 (6) | 0.1653 (4) | 0.075 (2) | |
C20 | 0.5108 (6) | −0.0267 (5) | 0.3502 (3) | 0.0628 (18) | |
C21 | 0.5020 (8) | −0.0879 (6) | 0.3027 (4) | 0.098 (3) | |
C30 | 0.7839 (6) | 0.9970 (6) | −0.0114 (3) | 0.0682 (19) | |
C31 | 0.8925 (7) | 1.0264 (8) | −0.0446 (5) | 0.112 (3) | |
C41 | 0.0395 (8) | 0.2719 (11) | 0.5423 (7) | 0.145 (5) | |
C42 | −0.0131 (12) | 0.3673 (10) | 0.5567 (8) | 0.217 (8) | |
H42A | 0.0287 | 0.4015 | 0.5789 | 0.325* | |
H42B | −0.0833 | 0.3519 | 0.5794 | 0.325* | |
H42C | −0.0201 | 0.4126 | 0.5215 | 0.325* | |
C51 | 0.4021 (12) | 0.6110 (12) | 0.2449 (6) | 0.141 (5) | |
C52 | 0.4366 (10) | 0.5150 (11) | 0.2266 (6) | 0.165 (5) | |
H52A | 0.4744 | 0.4762 | 0.2548 | 0.247* | |
H52B | 0.4839 | 0.5271 | 0.1896 | 0.247* | |
H52C | 0.3754 | 0.4758 | 0.2229 | 0.247* | |
C101 | 0.3927 (5) | 0.2571 (5) | 0.5497 (3) | 0.0533 (16) | |
C102 | 0.4727 (6) | 0.3309 (6) | 0.5395 (4) | 0.076 (2) | |
H102 | 0.5203 | 0.3383 | 0.5041 | 0.092* | |
C103 | 0.4833 (9) | 0.3944 (7) | 0.5812 (5) | 0.107 (3) | |
H103 | 0.5376 | 0.4441 | 0.5738 | 0.128* | |
C104 | 0.4138 (11) | 0.3837 (8) | 0.6330 (5) | 0.117 (4) | |
H104 | 0.4206 | 0.4265 | 0.6610 | 0.141* | |
C105 | 0.3350 (10) | 0.3115 (8) | 0.6441 (4) | 0.113 (4) | |
H105 | 0.2886 | 0.3044 | 0.6799 | 0.136* | |
C106 | 0.3223 (7) | 0.2474 (6) | 0.6027 (3) | 0.079 (2) | |
H106 | 0.2671 | 0.1986 | 0.6105 | 0.095* | |
C111 | 0.3247 (4) | 0.2610 (5) | 0.4393 (3) | 0.0474 (14) | |
C112 | 0.2922 (6) | 0.3621 (5) | 0.4446 (3) | 0.072 (2) | |
H112 | 0.3019 | 0.3911 | 0.4774 | 0.086* | |
C113 | 0.2456 (8) | 0.4216 (7) | 0.4026 (4) | 0.097 (3) | |
H113 | 0.2247 | 0.4904 | 0.4070 | 0.116* | |
C114 | 0.2298 (7) | 0.3810 (7) | 0.3546 (4) | 0.089 (3) | |
H114 | 0.1971 | 0.4214 | 0.3265 | 0.107* | |
C115 | 0.2621 (6) | 0.2801 (7) | 0.3476 (3) | 0.081 (2) | |
H115 | 0.2517 | 0.2520 | 0.3146 | 0.098* | |
C116 | 0.3100 (5) | 0.2203 (6) | 0.3896 (3) | 0.0638 (18) | |
H116 | 0.3326 | 0.1522 | 0.3845 | 0.077* | |
C201 | 0.8113 (5) | 0.0880 (5) | 0.4140 (3) | 0.0513 (15) | |
C202 | 0.8146 (5) | 0.0580 (6) | 0.3600 (3) | 0.070 (2) | |
H202 | 0.7657 | 0.0086 | 0.3555 | 0.085* | |
C203 | 0.8886 (6) | 0.0994 (8) | 0.3120 (3) | 0.088 (3) | |
H203 | 0.8887 | 0.0794 | 0.2755 | 0.105* | |
C204 | 0.9620 (7) | 0.1707 (7) | 0.3196 (4) | 0.093 (3) | |
H204 | 1.0133 | 0.1981 | 0.2881 | 0.112* | |
C205 | 0.9603 (7) | 0.2013 (7) | 0.3723 (5) | 0.097 (3) | |
H205 | 1.0098 | 0.2503 | 0.3767 | 0.116* | |
C206 | 0.8856 (5) | 0.1602 (5) | 0.4202 (4) | 0.075 (2) | |
H206 | 0.8854 | 0.1814 | 0.4565 | 0.090* | |
C211 | 0.7501 (5) | 0.0766 (5) | 0.5364 (3) | 0.0571 (16) | |
C212 | 0.7058 (6) | 0.1650 (7) | 0.5596 (3) | 0.082 (2) | |
H212 | 0.6509 | 0.2023 | 0.5440 | 0.098* | |
C213 | 0.7435 (9) | 0.1976 (10) | 0.6059 (5) | 0.122 (4) | |
H213 | 0.7154 | 0.2581 | 0.6207 | 0.146* | |
C214 | 0.8222 (12) | 0.1409 (13) | 0.6298 (5) | 0.142 (5) | |
H214 | 0.8483 | 0.1635 | 0.6606 | 0.170* | |
C215 | 0.8616 (10) | 0.0534 (10) | 0.6093 (6) | 0.133 (5) | |
H215 | 0.9124 | 0.0137 | 0.6272 | 0.159* | |
C216 | 0.8282 (7) | 0.0209 (7) | 0.5618 (4) | 0.094 (3) | |
H216 | 0.8586 | −0.0388 | 0.5470 | 0.112* | |
C301 | 0.5702 (5) | 0.6777 (5) | 0.0348 (3) | 0.0501 (15) | |
C302 | 0.5164 (6) | 0.5844 (5) | 0.0550 (3) | 0.0661 (19) | |
H302 | 0.4422 | 0.5818 | 0.0572 | 0.079* | |
C303 | 0.5733 (8) | 0.4945 (5) | 0.0719 (4) | 0.085 (2) | |
H303 | 0.5367 | 0.4322 | 0.0863 | 0.102* | |
C304 | 0.6824 (7) | 0.4970 (6) | 0.0674 (4) | 0.085 (3) | |
H304 | 0.7199 | 0.4366 | 0.0789 | 0.102* | |
C305 | 0.7369 (6) | 0.5884 (6) | 0.0459 (3) | 0.076 (2) | |
H305 | 0.8115 | 0.5895 | 0.0423 | 0.091* | |
C306 | 0.6817 (6) | 0.6791 (5) | 0.0294 (3) | 0.0634 (18) | |
H306 | 0.7191 | 0.7409 | 0.0148 | 0.076* | |
C311 | 0.3612 (5) | 0.7615 (4) | 0.0296 (3) | 0.0515 (15) | |
C312 | 0.3040 (5) | 0.7466 (5) | −0.0132 (3) | 0.0661 (19) | |
H312 | 0.3367 | 0.7576 | −0.0522 | 0.079* | |
C313 | 0.1983 (6) | 0.7155 (7) | 0.0018 (5) | 0.097 (3) | |
H313 | 0.1592 | 0.7077 | −0.0273 | 0.116* | |
C314 | 0.1499 (8) | 0.6958 (8) | 0.0595 (6) | 0.119 (4) | |
H314 | 0.0795 | 0.6716 | 0.0694 | 0.143* | |
C315 | 0.2065 (8) | 0.7121 (7) | 0.1023 (5) | 0.102 (3) | |
H315 | 0.1739 | 0.7003 | 0.1413 | 0.122* | |
C316 | 0.3107 (6) | 0.7458 (6) | 0.0876 (3) | 0.076 (2) | |
H316 | 0.3480 | 0.7584 | 0.1167 | 0.091* | |
C401 | 0.5296 (5) | 1.1065 (4) | 0.1584 (2) | 0.0456 (14) | |
C402 | 0.4725 (6) | 1.1570 (5) | 0.2028 (3) | 0.0623 (18) | |
H402 | 0.3992 | 1.1696 | 0.2043 | 0.075* | |
C403 | 0.5230 (7) | 1.1889 (6) | 0.2450 (3) | 0.076 (2) | |
H403 | 0.4834 | 1.2228 | 0.2745 | 0.091* | |
C404 | 0.6312 (7) | 1.1710 (6) | 0.2436 (3) | 0.077 (2) | |
H404 | 0.6650 | 1.1917 | 0.2722 | 0.092* | |
C405 | 0.6888 (6) | 1.1224 (6) | 0.1996 (3) | 0.075 (2) | |
H405 | 0.7624 | 1.1111 | 0.1980 | 0.090* | |
C406 | 0.6389 (5) | 1.0901 (5) | 0.1575 (3) | 0.0586 (17) | |
H406 | 0.6792 | 1.0568 | 0.1281 | 0.070* | |
C411 | 0.3323 (5) | 1.0332 (5) | 0.1416 (3) | 0.0475 (14) | |
C412 | 0.3216 (6) | 0.9401 (5) | 0.1783 (3) | 0.0661 (18) | |
H412 | 0.3815 | 0.8969 | 0.1811 | 0.079* | |
C413 | 0.2230 (7) | 0.9098 (7) | 0.2112 (3) | 0.084 (2) | |
H413 | 0.2163 | 0.8461 | 0.2355 | 0.101* | |
C414 | 0.1349 (7) | 0.9742 (8) | 0.2076 (4) | 0.096 (3) | |
H414 | 0.0683 | 0.9541 | 0.2297 | 0.116* | |
C415 | 0.1446 (6) | 1.0670 (8) | 0.1721 (4) | 0.096 (3) | |
H415 | 0.0848 | 1.1110 | 0.1708 | 0.115* | |
C416 | 0.2433 (5) | 1.0976 (6) | 0.1373 (3) | 0.0687 (19) | |
H416 | 0.2491 | 1.1599 | 0.1118 | 0.082* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mo | 0.0402 (3) | 0.0422 (3) | 0.0438 (3) | −0.0020 (2) | −0.0056 (2) | 0.0025 (2) |
Cu1 | 0.0398 (4) | 0.0508 (4) | 0.0463 (4) | 0.0035 (3) | −0.0028 (3) | −0.0071 (3) |
Cu2 | 0.0449 (4) | 0.0492 (4) | 0.0493 (4) | 0.0069 (3) | −0.0074 (3) | −0.0171 (3) |
P1 | 0.0386 (8) | 0.0396 (8) | 0.0462 (9) | 0.0007 (6) | −0.0007 (7) | −0.0036 (7) |
P2 | 0.0375 (8) | 0.0420 (8) | 0.0483 (9) | −0.0021 (6) | −0.0016 (7) | 0.0018 (7) |
P3 | 0.0435 (8) | 0.0410 (8) | 0.0439 (9) | 0.0069 (6) | −0.0084 (7) | −0.0105 (7) |
P4 | 0.0379 (8) | 0.0463 (8) | 0.0387 (8) | 0.0053 (6) | −0.0067 (6) | −0.0124 (7) |
S1 | 0.0429 (9) | 0.0757 (11) | 0.0578 (10) | 0.0063 (8) | −0.0118 (8) | −0.0169 (8) |
S2 | 0.0439 (9) | 0.0541 (9) | 0.0654 (10) | 0.0040 (7) | −0.0165 (8) | −0.0094 (8) |
S3 | 0.0659 (11) | 0.0599 (10) | 0.0485 (9) | −0.0154 (8) | −0.0110 (8) | 0.0000 (8) |
S4 | 0.0644 (10) | 0.0517 (9) | 0.0538 (10) | −0.0194 (8) | −0.0105 (8) | 0.0060 (7) |
S5 | 0.0392 (8) | 0.0486 (9) | 0.0871 (13) | −0.0060 (7) | −0.0124 (8) | 0.0098 (8) |
S6 | 0.0430 (8) | 0.0461 (8) | 0.0653 (10) | −0.0012 (7) | −0.0160 (7) | −0.0050 (7) |
N1 | 0.053 (4) | 0.098 (5) | 0.138 (6) | 0.015 (4) | −0.019 (4) | −0.047 (5) |
N2 | 0.074 (5) | 0.124 (6) | 0.115 (6) | 0.024 (4) | −0.022 (4) | −0.064 (5) |
N3 | 0.168 (8) | 0.091 (5) | 0.055 (4) | −0.015 (5) | −0.011 (5) | −0.008 (4) |
N4 | 0.063 (4) | 0.052 (3) | 0.065 (4) | −0.001 (3) | 0.005 (3) | 0.011 (3) |
N5 | 0.053 (4) | 0.059 (4) | 0.217 (9) | −0.004 (3) | −0.001 (5) | 0.031 (5) |
N6 | 0.073 (4) | 0.060 (3) | 0.067 (4) | 0.013 (3) | −0.027 (3) | −0.011 (3) |
N10 | 0.035 (3) | 0.045 (3) | 0.077 (4) | 0.002 (2) | 0.011 (2) | 0.000 (3) |
N11 | 0.059 (3) | 0.061 (3) | 0.052 (3) | 0.001 (3) | −0.007 (3) | −0.012 (3) |
N13 | 0.058 (4) | 0.063 (4) | 0.063 (4) | −0.001 (3) | −0.001 (3) | −0.013 (3) |
N20 | 0.050 (3) | 0.045 (3) | 0.041 (3) | 0.014 (2) | −0.007 (2) | −0.014 (2) |
N40 | 0.078 (7) | 0.128 (9) | 0.45 (2) | 0.044 (6) | 0.053 (10) | 0.025 (12) |
N50 | 0.39 (2) | 0.178 (14) | 0.250 (17) | 0.104 (15) | −0.131 (16) | −0.090 (13) |
C1 | 0.053 (4) | 0.081 (5) | 0.082 (5) | 0.016 (4) | −0.020 (4) | −0.029 (4) |
C2 | 0.046 (4) | 0.060 (4) | 0.061 (4) | 0.010 (3) | −0.008 (3) | −0.010 (3) |
C3 | 0.045 (4) | 0.052 (4) | 0.063 (4) | 0.005 (3) | −0.009 (3) | −0.004 (3) |
C4 | 0.048 (4) | 0.065 (4) | 0.093 (6) | 0.014 (3) | −0.021 (4) | −0.024 (4) |
C5 | 0.063 (4) | 0.044 (3) | 0.048 (4) | 0.004 (3) | 0.000 (3) | 0.008 (3) |
C6 | 0.054 (4) | 0.038 (3) | 0.057 (4) | −0.001 (3) | −0.001 (3) | 0.005 (3) |
C7 | 0.064 (4) | 0.050 (4) | 0.042 (4) | 0.002 (3) | −0.002 (3) | 0.002 (3) |
C8 | 0.097 (6) | 0.056 (4) | 0.049 (4) | −0.009 (4) | −0.003 (4) | −0.001 (3) |
C9 | 0.053 (4) | 0.049 (4) | 0.050 (4) | 0.000 (3) | −0.011 (3) | −0.007 (3) |
C10 | 0.040 (3) | 0.046 (3) | 0.050 (4) | 0.002 (3) | −0.006 (3) | 0.000 (3) |
C11 | 0.046 (4) | 0.045 (3) | 0.060 (4) | 0.001 (3) | 0.000 (3) | 0.011 (3) |
C12 | 0.039 (4) | 0.054 (4) | 0.120 (7) | 0.001 (3) | −0.004 (4) | 0.017 (4) |
C20 | 0.066 (5) | 0.062 (4) | 0.058 (4) | 0.004 (3) | −0.009 (4) | −0.006 (4) |
C21 | 0.153 (9) | 0.079 (6) | 0.071 (5) | −0.009 (5) | −0.028 (5) | −0.035 (4) |
C30 | 0.064 (5) | 0.065 (5) | 0.076 (5) | 0.002 (4) | −0.010 (4) | −0.014 (4) |
C31 | 0.056 (5) | 0.128 (8) | 0.140 (9) | −0.017 (5) | 0.020 (5) | −0.028 (7) |
C41 | 0.062 (6) | 0.120 (10) | 0.251 (16) | 0.011 (6) | −0.043 (8) | 0.000 (10) |
C42 | 0.205 (16) | 0.129 (11) | 0.37 (2) | 0.034 (11) | −0.140 (16) | −0.099 (14) |
C51 | 0.175 (13) | 0.132 (11) | 0.127 (10) | 0.003 (10) | −0.041 (9) | −0.039 (9) |
C52 | 0.150 (11) | 0.183 (13) | 0.165 (12) | −0.054 (10) | 0.020 (9) | −0.082 (10) |
C101 | 0.060 (4) | 0.046 (3) | 0.055 (4) | 0.020 (3) | −0.012 (3) | −0.010 (3) |
C102 | 0.075 (5) | 0.066 (5) | 0.096 (6) | 0.006 (4) | −0.022 (4) | −0.030 (4) |
C103 | 0.125 (8) | 0.088 (7) | 0.129 (9) | 0.017 (6) | −0.054 (7) | −0.055 (6) |
C104 | 0.185 (13) | 0.085 (7) | 0.107 (9) | 0.067 (8) | −0.076 (9) | −0.050 (7) |
C105 | 0.174 (11) | 0.090 (7) | 0.071 (6) | 0.054 (7) | −0.010 (7) | −0.025 (6) |
C106 | 0.101 (6) | 0.076 (5) | 0.057 (5) | 0.026 (4) | −0.004 (4) | −0.016 (4) |
C111 | 0.037 (3) | 0.050 (4) | 0.051 (4) | 0.002 (3) | −0.003 (3) | 0.002 (3) |
C112 | 0.079 (5) | 0.058 (4) | 0.080 (5) | 0.018 (4) | −0.024 (4) | −0.003 (4) |
C113 | 0.123 (8) | 0.071 (5) | 0.098 (7) | 0.034 (5) | −0.042 (6) | 0.005 (5) |
C114 | 0.085 (6) | 0.095 (7) | 0.081 (6) | 0.022 (5) | −0.023 (5) | 0.020 (5) |
C115 | 0.078 (5) | 0.105 (7) | 0.064 (5) | 0.013 (5) | −0.026 (4) | −0.005 (4) |
C116 | 0.061 (4) | 0.069 (5) | 0.060 (4) | 0.008 (4) | −0.011 (3) | −0.007 (4) |
C201 | 0.038 (3) | 0.052 (4) | 0.056 (4) | 0.006 (3) | −0.001 (3) | 0.010 (3) |
C202 | 0.044 (4) | 0.095 (6) | 0.068 (5) | −0.009 (4) | −0.005 (3) | 0.000 (4) |
C203 | 0.056 (5) | 0.137 (8) | 0.057 (5) | 0.009 (5) | 0.003 (4) | 0.015 (5) |
C204 | 0.058 (5) | 0.098 (7) | 0.096 (7) | 0.006 (5) | 0.024 (5) | 0.030 (5) |
C205 | 0.070 (5) | 0.083 (6) | 0.122 (8) | −0.028 (4) | 0.030 (5) | −0.012 (6) |
C206 | 0.057 (4) | 0.062 (4) | 0.095 (6) | −0.021 (4) | 0.015 (4) | −0.010 (4) |
C211 | 0.054 (4) | 0.062 (4) | 0.050 (4) | −0.015 (3) | −0.007 (3) | 0.009 (3) |
C212 | 0.074 (5) | 0.113 (7) | 0.062 (5) | 0.003 (5) | −0.011 (4) | −0.029 (5) |
C213 | 0.120 (9) | 0.165 (11) | 0.091 (7) | −0.020 (8) | −0.017 (7) | −0.053 (7) |
C214 | 0.173 (13) | 0.187 (14) | 0.077 (7) | −0.076 (12) | −0.055 (8) | −0.001 (8) |
C215 | 0.155 (11) | 0.121 (9) | 0.139 (11) | −0.037 (9) | −0.100 (9) | 0.030 (8) |
C216 | 0.094 (6) | 0.084 (6) | 0.115 (7) | −0.010 (5) | −0.064 (6) | 0.009 (5) |
C301 | 0.058 (4) | 0.048 (4) | 0.048 (4) | 0.014 (3) | −0.015 (3) | −0.020 (3) |
C302 | 0.075 (5) | 0.047 (4) | 0.084 (5) | 0.006 (3) | −0.030 (4) | −0.017 (4) |
C303 | 0.114 (7) | 0.043 (4) | 0.109 (7) | 0.005 (4) | −0.050 (6) | −0.012 (4) |
C304 | 0.109 (7) | 0.055 (5) | 0.108 (7) | 0.036 (5) | −0.058 (6) | −0.030 (4) |
C305 | 0.072 (5) | 0.075 (5) | 0.090 (6) | 0.027 (4) | −0.035 (4) | −0.026 (4) |
C306 | 0.069 (5) | 0.056 (4) | 0.066 (4) | 0.014 (3) | −0.014 (4) | −0.010 (3) |
C311 | 0.047 (4) | 0.042 (3) | 0.065 (4) | 0.003 (3) | −0.009 (3) | −0.009 (3) |
C312 | 0.056 (4) | 0.065 (4) | 0.080 (5) | −0.004 (3) | −0.007 (4) | −0.027 (4) |
C313 | 0.057 (5) | 0.104 (7) | 0.144 (9) | −0.009 (5) | −0.018 (5) | −0.060 (6) |
C314 | 0.064 (6) | 0.109 (8) | 0.180 (12) | −0.027 (5) | 0.025 (7) | −0.058 (8) |
C315 | 0.085 (6) | 0.097 (7) | 0.109 (8) | −0.024 (5) | 0.032 (6) | −0.024 (6) |
C316 | 0.067 (5) | 0.088 (5) | 0.068 (5) | −0.009 (4) | 0.009 (4) | −0.017 (4) |
C401 | 0.048 (3) | 0.046 (3) | 0.046 (3) | 0.001 (3) | −0.010 (3) | −0.014 (3) |
C402 | 0.069 (4) | 0.069 (4) | 0.054 (4) | 0.004 (4) | −0.012 (3) | −0.023 (3) |
C403 | 0.093 (6) | 0.076 (5) | 0.065 (5) | 0.001 (4) | −0.012 (4) | −0.033 (4) |
C404 | 0.101 (6) | 0.071 (5) | 0.072 (5) | −0.017 (4) | −0.035 (5) | −0.030 (4) |
C405 | 0.062 (5) | 0.088 (5) | 0.086 (6) | −0.002 (4) | −0.031 (4) | −0.025 (5) |
C406 | 0.054 (4) | 0.067 (4) | 0.061 (4) | −0.002 (3) | −0.017 (3) | −0.022 (3) |
C411 | 0.043 (3) | 0.058 (4) | 0.045 (3) | 0.003 (3) | −0.005 (3) | −0.020 (3) |
C412 | 0.065 (4) | 0.067 (5) | 0.061 (4) | −0.004 (4) | 0.001 (4) | −0.006 (4) |
C413 | 0.084 (6) | 0.098 (6) | 0.060 (5) | −0.018 (5) | 0.012 (4) | −0.005 (4) |
C414 | 0.060 (5) | 0.134 (8) | 0.084 (6) | −0.016 (5) | 0.017 (4) | −0.011 (6) |
C415 | 0.050 (5) | 0.127 (8) | 0.103 (7) | 0.016 (5) | 0.002 (5) | −0.010 (6) |
C416 | 0.050 (4) | 0.082 (5) | 0.070 (5) | 0.011 (4) | −0.005 (4) | −0.005 (4) |
Mo—S1 | 2.3768 (17) | C111—C116 | 1.388 (9) |
Mo—S2 | 2.3990 (16) | C112—C113 | 1.370 (10) |
Mo—S3 | 2.3696 (17) | C112—H112 | 0.930 |
Mo—S4 | 2.3716 (16) | C113—C114 | 1.355 (11) |
Mo—S5 | 2.3980 (16) | C113—H113 | 0.930 |
Mo—S6 | 2.3916 (16) | C114—C115 | 1.371 (11) |
Cu1—P1 | 2.2590 (16) | C114—H114 | 0.930 |
Cu1—P2 | 2.2689 (17) | C115—C116 | 1.380 (9) |
Cu1—N4 | 2.176 (5) | C115—H115 | 0.930 |
Cu1—N11 | 2.033 (6) | C116—H116 | 0.930 |
Cu2—P3 | 2.2693 (16) | C201—C202 | 1.369 (9) |
Cu2—P4 | 2.2523 (15) | C201—C206 | 1.380 (9) |
Cu2—N6 | 2.171 (6) | C202—C203 | 1.386 (9) |
Cu2—N13 | 2.022 (6) | C202—H202 | 0.930 |
P1—N10i | 1.678 (5) | C203—C204 | 1.375 (12) |
P1—C101 | 1.821 (6) | C203—H203 | 0.930 |
P1—C111 | 1.842 (6) | C204—C205 | 1.347 (12) |
P2—N10 | 1.686 (5) | C204—H204 | 0.930 |
P2—C211 | 1.813 (7) | C205—C206 | 1.387 (10) |
P2—C201 | 1.835 (6) | C205—H205 | 0.930 |
P3—N20 | 1.693 (5) | C206—H206 | 0.930 |
P3—C301 | 1.821 (6) | C211—C216 | 1.373 (9) |
P3—C311 | 1.829 (6) | C211—C212 | 1.387 (10) |
P4—N20ii | 1.681 (5) | C212—C213 | 1.382 (11) |
P4—C401 | 1.817 (6) | C212—H212 | 0.930 |
P4—C411 | 1.827 (6) | C213—C214 | 1.370 (16) |
S1—C2 | 1.731 (6) | C213—H213 | 0.930 |
S2—C3 | 1.723 (7) | C214—C215 | 1.332 (16) |
S3—C7 | 1.741 (6) | C214—H214 | 0.930 |
S4—C6 | 1.718 (6) | C215—C216 | 1.382 (13) |
S5—C11 | 1.732 (6) | C215—H215 | 0.930 |
S6—C10 | 1.712 (6) | C216—H216 | 0.930 |
N1—C4 | 1.147 (8) | C301—C302 | 1.382 (9) |
N2—C1 | 1.135 (9) | C301—C306 | 1.391 (9) |
N3—C8 | 1.143 (8) | C302—C303 | 1.390 (9) |
N4—C5 | 1.138 (7) | C302—H302 | 0.930 |
N5—C12 | 1.140 (8) | C303—C304 | 1.363 (11) |
N6—C9 | 1.151 (7) | C303—H303 | 0.930 |
N10—P1i | 1.678 (5) | C304—C305 | 1.371 (11) |
N10—H10 | 0.860 | C304—H304 | 0.930 |
N11—C20 | 1.140 (8) | C305—C306 | 1.384 (9) |
N13—C30 | 1.123 (8) | C305—H305 | 0.930 |
N20—P4ii | 1.681 (5) | C306—H306 | 0.930 |
N20—H20 | 0.860 | C311—C312 | 1.375 (9) |
N40—C41 | 1.047 (14) | C311—C316 | 1.387 (9) |
N50—C51 | 1.086 (15) | C312—C313 | 1.376 (10) |
C1—C2 | 1.426 (9) | C312—H312 | 0.930 |
C2—C3 | 1.353 (8) | C313—C314 | 1.377 (13) |
C3—C4 | 1.438 (9) | C313—H313 | 0.930 |
C5—C6 | 1.430 (8) | C314—C315 | 1.375 (13) |
C6—C7 | 1.348 (9) | C314—H314 | 0.930 |
C7—C8 | 1.407 (9) | C315—C316 | 1.368 (11) |
C9—C10 | 1.417 (8) | C315—H315 | 0.930 |
C10—C11 | 1.363 (8) | C316—H316 | 0.930 |
C11—C12 | 1.426 (9) | C401—C402 | 1.385 (8) |
C20—C21 | 1.474 (10) | C401—C406 | 1.385 (8) |
C30—C31 | 1.483 (11) | C402—C403 | 1.384 (9) |
C41—C42 | 1.430 (16) | C402—H402 | 0.930 |
C42—H42A | 0.960 | C403—C404 | 1.372 (10) |
C42—H42B | 0.960 | C403—H403 | 0.930 |
C42—H42C | 0.960 | C404—C405 | 1.368 (10) |
C51—C52 | 1.395 (16) | C404—H404 | 0.930 |
C52—H52A | 0.960 | C405—C406 | 1.377 (9) |
C52—H52B | 0.960 | C405—H405 | 0.930 |
C52—H52C | 0.960 | C406—H406 | 0.930 |
C101—C102 | 1.376 (9) | C411—C412 | 1.372 (9) |
C101—C106 | 1.387 (9) | C411—C416 | 1.383 (8) |
C102—C103 | 1.386 (11) | C412—C413 | 1.379 (9) |
C102—H102 | 0.930 | C412—H412 | 0.930 |
C103—C104 | 1.360 (14) | C413—C414 | 1.373 (11) |
C103—H103 | 0.930 | C413—H413 | 0.930 |
C104—C105 | 1.350 (14) | C414—C415 | 1.356 (12) |
C104—H104 | 0.930 | C414—H414 | 0.930 |
C105—C106 | 1.393 (12) | C415—C416 | 1.399 (10) |
C105—H105 | 0.930 | C415—H415 | 0.930 |
C106—H106 | 0.930 | C416—H416 | 0.930 |
C111—C112 | 1.367 (8) | ||
S1—Mo—S2 | 81.74 (6) | C112—C111—P1 | 124.7 (5) |
S1—Mo—S3 | 147.56 (6) | C116—C111—P1 | 117.3 (5) |
S1—Mo—S4 | 80.92 (6) | C111—C112—C113 | 121.3 (8) |
S1—Mo—S5 | 120.19 (7) | C111—C112—H112 | 119.3 |
S1—Mo—S6 | 86.21 (6) | C113—C112—H112 | 119.3 |
S2—Mo—S3 | 84.39 (6) | C114—C113—C112 | 120.5 (8) |
S2—Mo—S4 | 123.34 (6) | C114—C113—H113 | 119.7 |
S2—Mo—S5 | 82.94 (6) | C112—C113—H113 | 119.7 |
S2—Mo—S6 | 151.98 (6) | C113—C114—C115 | 119.8 (7) |
S3—Mo—S4 | 82.52 (6) | C113—C114—H114 | 120.1 |
S3—Mo—S5 | 86.76 (6) | C115—C114—H114 | 120.1 |
S3—Mo—S6 | 117.66 (6) | C114—C115—C116 | 119.8 (8) |
S4—Mo—S5 | 150.11 (6) | C114—C115—H115 | 120.1 |
S4—Mo—S6 | 79.06 (6) | C116—C115—H115 | 120.1 |
S5—Mo—S6 | 81.45 (5) | C115—C116—C111 | 120.6 (7) |
P1—Cu1—P2 | 140.00 (7) | C115—C116—H116 | 119.7 |
P1—Cu1—N4 | 95.21 (15) | C111—C116—H116 | 119.7 |
P1—Cu1—N11 | 112.36 (16) | C202—C201—C206 | 118.3 (6) |
P2—Cu1—N4 | 96.02 (15) | C202—C201—P2 | 119.3 (5) |
P2—Cu1—N11 | 102.91 (16) | C206—C201—P2 | 122.1 (5) |
N4—Cu1—N11 | 101.0 (2) | C201—C202—C203 | 121.8 (7) |
P3—Cu2—P4 | 134.42 (6) | C201—C202—H202 | 119.1 |
P3—Cu2—N6 | 100.43 (15) | C203—C202—H202 | 119.1 |
P3—Cu2—N13 | 105.12 (16) | C204—C203—C202 | 118.5 (8) |
P4—Cu2—N6 | 101.58 (15) | C204—C203—H203 | 120.7 |
P4—Cu2—N13 | 112.63 (16) | C202—C203—H203 | 120.7 |
N6—Cu2—N13 | 93.8 (2) | C205—C204—C203 | 120.7 (8) |
N10i—P1—C101 | 104.8 (3) | C205—C204—H204 | 119.7 |
N10i—P1—C111 | 102.7 (3) | C203—C204—H204 | 119.7 |
C101—P1—C111 | 103.0 (3) | C204—C205—C206 | 120.6 (8) |
N10i—P1—Cu1 | 116.54 (18) | C204—C205—H205 | 119.7 |
C101—P1—Cu1 | 117.5 (2) | C206—C205—H205 | 119.7 |
C111—P1—Cu1 | 110.47 (19) | C201—C206—C205 | 120.1 (8) |
N10—P2—C211 | 106.9 (3) | C201—C206—H206 | 119.9 |
N10—P2—C201 | 101.8 (3) | C205—C206—H206 | 119.9 |
C211—P2—C201 | 101.5 (3) | C216—C211—C212 | 118.8 (7) |
N10—P2—Cu1 | 113.03 (19) | C216—C211—P2 | 123.7 (6) |
C211—P2—Cu1 | 121.2 (2) | C212—C211—P2 | 117.5 (5) |
C201—P2—Cu1 | 110.15 (19) | C213—C212—C211 | 119.8 (9) |
N20—P3—C301 | 100.9 (2) | C213—C212—H212 | 120.1 |
N20—P3—C311 | 107.8 (3) | C211—C212—H212 | 120.1 |
C301—P3—C311 | 101.8 (3) | C214—C213—C212 | 119.9 (11) |
N20—P3—Cu2 | 112.21 (17) | C214—C213—H213 | 120.0 |
C301—P3—Cu2 | 112.2 (2) | C212—C213—H213 | 120.0 |
C311—P3—Cu2 | 119.9 (2) | C215—C214—C213 | 120.3 (11) |
N20ii—P4—C401 | 102.1 (2) | C215—C214—H214 | 119.8 |
N20ii—P4—C411 | 107.0 (3) | C213—C214—H214 | 119.8 |
C401—P4—C411 | 100.5 (3) | C214—C215—C216 | 121.0 (11) |
N20ii—P4—Cu2 | 117.12 (16) | C214—C215—H215 | 119.5 |
C401—P4—Cu2 | 113.94 (19) | C216—C215—H215 | 119.5 |
C411—P4—Cu2 | 114.2 (2) | C211—C216—C215 | 120.0 (10) |
C2—S1—Mo | 108.8 (2) | C211—C216—H216 | 120.0 |
C3—S2—Mo | 107.7 (2) | C215—C216—H216 | 120.0 |
C7—S3—Mo | 107.6 (2) | C302—C301—C306 | 119.2 (6) |
C6—S4—Mo | 107.8 (2) | C302—C301—P3 | 123.3 (5) |
C11—S5—Mo | 108.1 (2) | C306—C301—P3 | 117.5 (5) |
C10—S6—Mo | 108.7 (2) | C301—C302—C303 | 119.9 (7) |
C5—N4—Cu1 | 158.1 (5) | C301—C302—H302 | 120.0 |
C9—N6—Cu2 | 153.1 (5) | C303—C302—H302 | 120.0 |
P1i—N10—P2 | 123.6 (3) | C304—C303—C302 | 120.5 (8) |
P1i—N10—H10 | 118.2 | C304—C303—H303 | 119.8 |
P2—N10—H10 | 118.2 | C302—C303—H303 | 119.8 |
C20—N11—Cu1 | 178.0 (6) | C303—C304—C305 | 120.1 (7) |
C30—N13—Cu2 | 179.0 (7) | C303—C304—H304 | 120.0 |
P4ii—N20—P3 | 124.7 (3) | C305—C304—H304 | 120.0 |
P4ii—N20—H20 | 117.7 | C304—C305—C306 | 120.4 (7) |
P3—N20—H20 | 117.7 | C304—C305—H305 | 119.8 |
N2—C1—C2 | 176.3 (8) | C306—C305—H305 | 119.8 |
C3—C2—C1 | 123.6 (6) | C305—C306—C301 | 119.9 (7) |
C3—C2—S1 | 120.1 (5) | C305—C306—H306 | 120.0 |
C1—C2—S1 | 116.3 (5) | C301—C306—H306 | 120.0 |
C2—C3—C4 | 121.2 (6) | C312—C311—C316 | 119.2 (6) |
C2—C3—S2 | 121.6 (5) | C312—C311—P3 | 123.9 (5) |
C4—C3—S2 | 117.2 (5) | C316—C311—P3 | 116.9 (5) |
N1—C4—C3 | 178.4 (8) | C311—C312—C313 | 119.9 (8) |
N4—C5—C6 | 176.7 (7) | C311—C312—H312 | 120.0 |
C7—C6—C5 | 122.8 (6) | C313—C312—H312 | 120.0 |
C7—C6—S4 | 121.5 (5) | C312—C313—C314 | 120.6 (9) |
C5—C6—S4 | 115.7 (5) | C312—C313—H313 | 119.7 |
C6—C7—C8 | 121.6 (6) | C314—C313—H313 | 119.7 |
C6—C7—S3 | 120.4 (5) | C315—C314—C313 | 119.5 (8) |
C8—C7—S3 | 118.0 (5) | C315—C314—H314 | 120.3 |
N3—C8—C7 | 178.4 (9) | C313—C314—H314 | 120.3 |
N6—C9—C10 | 179.1 (7) | C316—C315—C314 | 120.1 (9) |
C11—C10—C9 | 121.4 (5) | C316—C315—H315 | 120.0 |
C11—C10—S6 | 121.0 (4) | C314—C315—H315 | 120.0 |
C9—C10—S6 | 117.6 (4) | C315—C316—C311 | 120.6 (8) |
C10—C11—C12 | 122.1 (6) | C315—C316—H316 | 119.7 |
C10—C11—S5 | 120.5 (5) | C311—C316—H316 | 119.7 |
C12—C11—S5 | 117.3 (5) | C402—C401—C406 | 117.6 (6) |
N5—C12—C11 | 178.2 (10) | C402—C401—P4 | 122.4 (5) |
N11—C20—C21 | 178.7 (8) | C406—C401—P4 | 119.9 (4) |
N13—C30—C31 | 179.2 (10) | C403—C402—C401 | 121.0 (7) |
N40—C41—C42 | 176 (2) | C403—C402—H402 | 119.5 |
C41—C42—H42A | 109.5 | C401—C402—H402 | 119.5 |
C41—C42—H42B | 109.5 | C404—C403—C402 | 120.3 (7) |
H42A—C42—H42B | 109.5 | C404—C403—H403 | 119.8 |
C41—C42—H42C | 109.4 | C402—C403—H403 | 119.8 |
H42A—C42—H42C | 109.5 | C405—C404—C403 | 119.3 (7) |
H42B—C42—H42C | 109.5 | C405—C404—H404 | 120.3 |
N50—C51—C52 | 177.3 (19) | C403—C404—H404 | 120.3 |
C51—C52—H52A | 109.5 | C404—C405—C406 | 120.6 (7) |
C51—C52—H52B | 109.5 | C404—C405—H405 | 119.7 |
H52A—C52—H52B | 109.5 | C406—C405—H405 | 119.7 |
C51—C52—H52C | 109.5 | C405—C406—C401 | 121.2 (6) |
H52A—C52—H52C | 109.5 | C405—C406—H406 | 119.4 |
H52B—C52—H52C | 109.5 | C401—C406—H406 | 119.4 |
C102—C101—C106 | 118.7 (7) | C412—C411—C416 | 119.8 (6) |
C102—C101—P1 | 118.7 (5) | C412—C411—P4 | 116.9 (5) |
C106—C101—P1 | 122.5 (6) | C416—C411—P4 | 123.3 (5) |
C101—C102—C103 | 120.9 (9) | C411—C412—C413 | 120.8 (7) |
C101—C102—H102 | 119.5 | C411—C412—H412 | 119.6 |
C103—C102—H102 | 119.5 | C413—C412—H412 | 119.6 |
C104—C103—C102 | 119.7 (10) | C414—C413—C412 | 119.6 (8) |
C104—C103—H103 | 120.2 | C414—C413—H413 | 120.2 |
C102—C103—H103 | 120.2 | C412—C413—H413 | 120.2 |
C105—C104—C103 | 120.5 (10) | C415—C414—C413 | 120.3 (8) |
C105—C104—H104 | 119.8 | C415—C414—H414 | 119.9 |
C103—C104—H104 | 119.8 | C413—C414—H414 | 119.9 |
C104—C105—C106 | 120.9 (10) | C414—C415—C416 | 120.8 (8) |
C104—C105—H105 | 119.6 | C414—C415—H415 | 119.6 |
C106—C105—H105 | 119.6 | C416—C415—H415 | 119.6 |
C101—C106—C105 | 119.4 (9) | C411—C416—C415 | 118.7 (7) |
C101—C106—H106 | 120.3 | C411—C416—H416 | 120.7 |
C105—C106—H106 | 120.3 | C415—C416—H416 | 120.7 |
C112—C111—C116 | 118.0 (6) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, −y+2, −z. |