Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108767311011883/sh5129sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108767311011883/sh5129Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108767311011883/sh5129sup3.pdf |
CCDC reference: 841921
Data collection: Bruker APEX2; cell refinement: Bruker SAINT; data reduction: Bruker SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
C20H60N4O16P8Rh2·2(C24H20B) | F(000) = 3536 |
Mr = 1704.72 | Dx = 1.425 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.9783 (3) Å | Cell parameters from 14691 reflections |
b = 20.2046 (5) Å | θ = 1.2–27.0° |
c = 28.1465 (7) Å | µ = 0.64 mm−1 |
β = 90.842 (1)° | T = 225 K |
V = 7948.4 (3) Å3 | Prismatic, red |
Z = 4 | 0.31 × 0.18 × 0.10 mm |
Bruker APEX-II CCD diffractometer | 17345 independent reflections |
Radiation source: RIGAKU rotating anode | 14691 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.000 |
ϕ and ω scans | θmax = 27.0°, θmin = 1.2° |
Absorption correction: numerical BRUKER SADABS | h = −17→17 |
Tmin = 0.826, Tmax = 0.939 | k = 0→25 |
17345 measured reflections | l = 0→35 |
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)] = 0.030 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.081 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0311P)2 + 6.6036P] where P = (Fo2 + 2Fc2)/3 |
17345 reflections | (Δ/σ)max = 0.001 |
905 parameters | Δρmax = 1.12 e Å−3 |
0 restraints | Δρmin = −0.40 e Å−3 |
C20H60N4O16P8Rh2·2(C24H20B) | V = 7948.4 (3) Å3 |
Mr = 1704.72 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 13.9783 (3) Å | µ = 0.64 mm−1 |
b = 20.2046 (5) Å | T = 225 K |
c = 28.1465 (7) Å | 0.31 × 0.18 × 0.10 mm |
β = 90.842 (1)° |
Bruker APEX-II CCD diffractometer | 17345 independent reflections |
Absorption correction: numerical BRUKER SADABS | 14691 reflections with I > 2σ(I) |
Tmin = 0.826, Tmax = 0.939 | Rint = 0.000 |
17345 measured reflections |
R[F2 > 2σ(F2)] = 0.030 | 0 restraints |
wR(F2) = 0.081 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.12 e Å−3 |
17345 reflections | Δρmin = −0.40 e Å−3 |
905 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. |
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 | ||
C1 | 0.40916 (18) | 0.35330 (16) | 0.13648 (12) | 0.0557 (8) | |
H1A | 0.3601 | 0.3496 | 0.1119 | 0.084* | |
H1B | 0.3959 | 0.3914 | 0.1563 | 0.084* | |
H1C | 0.4094 | 0.3135 | 0.1558 | 0.084* | |
C2 | 0.5349 (3) | 0.49389 (15) | 0.16084 (13) | 0.0688 (9) | |
H2A | 0.5291 | 0.5255 | 0.1866 | 0.103* | |
H2B | 0.4722 | 0.4854 | 0.1469 | 0.103* | |
H2C | 0.5766 | 0.5118 | 0.1368 | 0.103* | |
C3 | 0.93105 (18) | 0.38238 (14) | 0.06004 (10) | 0.0472 (6) | |
H3A | 0.9484 | 0.4029 | 0.0302 | 0.071* | |
H3B | 0.9458 | 0.3355 | 0.0589 | 0.071* | |
H3C | 0.9668 | 0.4029 | 0.0859 | 0.071* | |
C4 | 0.8219 (2) | 0.47746 (13) | 0.15501 (12) | 0.0582 (8) | |
H4A | 0.8532 | 0.4963 | 0.1829 | 0.087* | |
H4B | 0.7549 | 0.4899 | 0.1546 | 0.087* | |
H4C | 0.8522 | 0.4941 | 0.1266 | 0.087* | |
C5 | 0.6448 (2) | 0.43172 (16) | 0.06363 (10) | 0.0541 (8) | |
H5A | 0.6621 | 0.4093 | 0.0345 | 0.081* | |
H5B | 0.6780 | 0.4738 | 0.0656 | 0.081* | |
H5C | 0.5762 | 0.4393 | 0.0636 | 0.081* | |
C6 | 0.6049 (2) | 0.07544 (13) | 0.13756 (11) | 0.0522 (7) | |
H6A | 0.6372 | 0.0379 | 0.1521 | 0.078* | |
H6B | 0.6226 | 0.0785 | 0.1044 | 0.078* | |
H6C | 0.5362 | 0.0696 | 0.1397 | 0.078* | |
C7 | 0.42909 (19) | 0.17813 (17) | 0.18806 (10) | 0.0534 (7) | |
H7A | 0.3612 | 0.1739 | 0.1811 | 0.080* | |
H7B | 0.4392 | 0.2122 | 0.2119 | 0.080* | |
H7C | 0.4536 | 0.1363 | 0.2000 | 0.080* | |
C8 | 0.7020 (2) | 0.12052 (16) | 0.00387 (10) | 0.0565 (8) | |
H8A | 0.7388 | 0.0813 | −0.0037 | 0.085* | |
H8B | 0.6985 | 0.1492 | −0.0238 | 0.085* | |
H8C | 0.6379 | 0.1077 | 0.0129 | 0.085* | |
C9 | 0.7620 (2) | 0.28391 (17) | −0.01143 (9) | 0.0532 (7) | |
H9A | 0.7367 | 0.3127 | −0.0362 | 0.080* | |
H9B | 0.7842 | 0.2430 | −0.0255 | 0.080* | |
H9C | 0.8149 | 0.3057 | 0.0048 | 0.080* | |
C10 | 0.51781 (17) | 0.19984 (15) | 0.05363 (9) | 0.0435 (6) | |
H10A | 0.4659 | 0.2290 | 0.0624 | 0.065* | |
H10B | 0.4969 | 0.1542 | 0.0560 | 0.065* | |
H10C | 0.5365 | 0.2091 | 0.0213 | 0.065* | |
C11 | 0.9785 (2) | 0.24800 (19) | 0.27245 (9) | 0.0613 (9) | |
H11A | 0.9487 | 0.2589 | 0.3024 | 0.092* | |
H11B | 1.0374 | 0.2729 | 0.2694 | 0.092* | |
H11C | 0.9926 | 0.2010 | 0.2717 | 0.092* | |
C12 | 1.05222 (19) | 0.35787 (13) | 0.18527 (10) | 0.0477 (6) | |
H12A | 1.1175 | 0.3709 | 0.1788 | 0.071* | |
H12B | 1.0397 | 0.3638 | 0.2188 | 0.071* | |
H12C | 1.0084 | 0.3851 | 0.1667 | 0.071* | |
C13 | 0.8718 (4) | 0.02134 (18) | 0.1312 (2) | 0.141 (3) | |
H13A | 0.8301 | −0.0100 | 0.1468 | 0.212* | |
H13B | 0.9375 | 0.0135 | 0.1413 | 0.212* | |
H13C | 0.8663 | 0.0158 | 0.0970 | 0.212* | |
C14 | 0.99257 (19) | 0.17595 (14) | 0.05140 (9) | 0.0450 (6) | |
H14A | 1.0270 | 0.1529 | 0.0267 | 0.067* | |
H14B | 1.0364 | 0.2044 | 0.0690 | 0.067* | |
H14C | 0.9422 | 0.2026 | 0.0370 | 0.067* | |
C15 | 1.0544 (2) | 0.13666 (14) | 0.18628 (11) | 0.0518 (7) | |
H15A | 1.0806 | 0.1120 | 0.1599 | 0.078* | |
H15B | 1.0356 | 0.1062 | 0.2111 | 0.078* | |
H15C | 1.1026 | 0.1669 | 0.1987 | 0.078* | |
C16 | 0.4763 (2) | 0.3616 (2) | 0.27901 (13) | 0.0739 (10) | |
H16A | 0.4300 | 0.3910 | 0.2933 | 0.111* | |
H16B | 0.4757 | 0.3193 | 0.2952 | 0.111* | |
H16C | 0.4598 | 0.3552 | 0.2457 | 0.111* | |
C17 | 0.8294 (2) | 0.40082 (19) | 0.27488 (14) | 0.0723 (10) | |
H17A | 0.8613 | 0.4413 | 0.2846 | 0.108* | |
H17B | 0.8479 | 0.3894 | 0.2428 | 0.108* | |
H17C | 0.8476 | 0.3653 | 0.2964 | 0.108* | |
C18 | 0.5622 (3) | 0.1560 (2) | 0.32156 (12) | 0.0822 (12) | |
H18A | 0.5025 | 0.1315 | 0.3207 | 0.123* | |
H18B | 0.5571 | 0.1925 | 0.3438 | 0.123* | |
H18C | 0.6138 | 0.1269 | 0.3316 | 0.123* | |
C19 | 0.7742 (2) | 0.11632 (16) | 0.25468 (11) | 0.0598 (8) | |
H19A | 0.8301 | 0.0948 | 0.2684 | 0.090* | |
H19B | 0.7842 | 0.1238 | 0.2211 | 0.090* | |
H19C | 0.7186 | 0.0883 | 0.2588 | 0.090* | |
C20 | 0.6993 (3) | 0.29074 (16) | 0.35101 (9) | 0.0606 (8) | |
H20A | 0.7278 | 0.3330 | 0.3595 | 0.091* | |
H20B | 0.7419 | 0.2552 | 0.3608 | 0.091* | |
H20C | 0.6385 | 0.2859 | 0.3668 | 0.091* | |
C21 | 0.24434 (16) | 0.28299 (11) | 0.03113 (9) | 0.0333 (5) | |
C22 | 0.22048 (18) | 0.27995 (13) | 0.07908 (9) | 0.0405 (6) | |
H22 | 0.2028 | 0.3193 | 0.0945 | 0.049* | |
C23 | 0.2217 (2) | 0.22166 (15) | 0.10503 (11) | 0.0537 (7) | |
H23 | 0.2051 | 0.2223 | 0.1373 | 0.064* | |
C24 | 0.2464 (2) | 0.16394 (15) | 0.08434 (12) | 0.0559 (8) | |
H24 | 0.2486 | 0.1247 | 0.1022 | 0.067* | |
C25 | 0.2684 (2) | 0.16306 (14) | 0.03711 (13) | 0.0575 (8) | |
H25 | 0.2838 | 0.1229 | 0.0222 | 0.069* | |
C26 | 0.2678 (2) | 0.22213 (13) | 0.01092 (11) | 0.0475 (6) | |
H26 | 0.2839 | 0.2207 | −0.0214 | 0.057* | |
C27 | 0.32680 (16) | 0.34652 (11) | −0.04053 (8) | 0.0305 (5) | |
C28 | 0.42136 (17) | 0.33183 (13) | −0.02628 (9) | 0.0402 (5) | |
H28 | 0.4348 | 0.3254 | 0.0062 | 0.048* | |
C29 | 0.49542 (18) | 0.32654 (14) | −0.05820 (10) | 0.0459 (6) | |
H29 | 0.5576 | 0.3168 | −0.0472 | 0.055* | |
C30 | 0.47828 (19) | 0.33553 (14) | −0.10604 (10) | 0.0463 (6) | |
H30 | 0.5282 | 0.3318 | −0.1279 | 0.056* | |
C31 | 0.3868 (2) | 0.35014 (14) | −0.12139 (9) | 0.0447 (6) | |
H31 | 0.3740 | 0.3561 | −0.1540 | 0.054* | |
C32 | 0.31312 (17) | 0.35609 (12) | −0.08889 (8) | 0.0358 (5) | |
H32 | 0.2516 | 0.3670 | −0.1002 | 0.043* | |
C33 | 0.13700 (16) | 0.35945 (11) | −0.02663 (8) | 0.0308 (5) | |
C34 | 0.07937 (17) | 0.30510 (12) | −0.03877 (8) | 0.0345 (5) | |
H34 | 0.1013 | 0.2624 | −0.0312 | 0.041* | |
C35 | −0.00921 (18) | 0.31190 (13) | −0.06167 (9) | 0.0406 (6) | |
H35 | −0.0453 | 0.2740 | −0.0693 | 0.049* | |
C36 | −0.04423 (17) | 0.37350 (13) | −0.07314 (9) | 0.0406 (6) | |
H36 | −0.1041 | 0.3782 | −0.0884 | 0.049* | |
C37 | 0.01023 (18) | 0.42825 (13) | −0.06178 (9) | 0.0433 (6) | |
H37 | −0.0128 | 0.4708 | −0.0693 | 0.052* | |
C38 | 0.09878 (17) | 0.42115 (12) | −0.03940 (9) | 0.0380 (5) | |
H38 | 0.1347 | 0.4594 | −0.0325 | 0.046* | |
C39 | 0.26314 (17) | 0.41729 (11) | 0.03337 (8) | 0.0345 (5) | |
C40 | 0.1969 (2) | 0.43726 (14) | 0.06751 (10) | 0.0473 (6) | |
H40 | 0.1390 | 0.4139 | 0.0698 | 0.057* | |
C41 | 0.2135 (2) | 0.49018 (17) | 0.09802 (11) | 0.0632 (9) | |
H41 | 0.1682 | 0.5008 | 0.1212 | 0.076* | |
C42 | 0.2954 (3) | 0.52690 (15) | 0.09452 (12) | 0.0650 (10) | |
H42 | 0.3066 | 0.5627 | 0.1152 | 0.078* | |
C43 | 0.3609 (2) | 0.51095 (14) | 0.06049 (11) | 0.0562 (8) | |
H43 | 0.4165 | 0.5366 | 0.0572 | 0.067* | |
C44 | 0.3449 (2) | 0.45677 (12) | 0.03090 (9) | 0.0423 (6) | |
H44 | 0.3912 | 0.4463 | 0.0082 | 0.051* | |
C45 | 0.71480 (16) | 0.16948 (11) | 0.82290 (8) | 0.0329 (5) | |
C46 | 0.7147 (2) | 0.23092 (13) | 0.84617 (10) | 0.0468 (6) | |
H46 | 0.7023 | 0.2322 | 0.8789 | 0.056* | |
C47 | 0.7323 (2) | 0.29040 (13) | 0.82239 (12) | 0.0558 (8) | |
H47 | 0.7320 | 0.3305 | 0.8393 | 0.067* | |
C48 | 0.7499 (2) | 0.29067 (14) | 0.77458 (12) | 0.0530 (7) | |
H48 | 0.7622 | 0.3306 | 0.7587 | 0.064* | |
C49 | 0.7494 (2) | 0.23211 (14) | 0.75040 (11) | 0.0471 (6) | |
H49 | 0.7602 | 0.2317 | 0.7175 | 0.057* | |
C50 | 0.73303 (16) | 0.17329 (12) | 0.77430 (9) | 0.0362 (5) | |
H50 | 0.7342 | 0.1337 | 0.7568 | 0.043* | |
C51 | 0.79779 (18) | 0.08350 (11) | 0.88335 (9) | 0.0367 (5) | |
C52 | 0.86476 (18) | 0.13093 (13) | 0.89733 (9) | 0.0399 (5) | |
H52 | 0.8571 | 0.1744 | 0.8860 | 0.048* | |
C53 | 0.9421 (2) | 0.11722 (16) | 0.92709 (10) | 0.0518 (7) | |
H53 | 0.9852 | 0.1512 | 0.9353 | 0.062* | |
C54 | 0.9564 (2) | 0.05458 (16) | 0.94477 (11) | 0.0606 (8) | |
H54 | 1.0079 | 0.0455 | 0.9656 | 0.073* | |
C55 | 0.8939 (3) | 0.00584 (16) | 0.93134 (14) | 0.0714 (10) | |
H55 | 0.9028 | −0.0375 | 0.9426 | 0.086* | |
C56 | 0.8173 (2) | 0.02011 (14) | 0.90103 (13) | 0.0631 (9) | |
H56 | 0.7763 | −0.0147 | 0.8919 | 0.076* | |
C57 | 0.68558 (18) | 0.04139 (11) | 0.80956 (8) | 0.0356 (5) | |
C58 | 0.7615 (2) | 0.00950 (13) | 0.78717 (11) | 0.0500 (7) | |
H58 | 0.8238 | 0.0149 | 0.7996 | 0.060* | |
C59 | 0.7478 (2) | −0.02989 (14) | 0.74726 (11) | 0.0585 (8) | |
H59 | 0.8008 | −0.0497 | 0.7328 | 0.070* | |
C60 | 0.6570 (2) | −0.04029 (13) | 0.72854 (10) | 0.0539 (7) | |
H60 | 0.6478 | −0.0667 | 0.7014 | 0.065* | |
C61 | 0.5804 (2) | −0.01115 (13) | 0.75046 (10) | 0.0493 (7) | |
H61 | 0.5180 | −0.0183 | 0.7386 | 0.059* | |
C62 | 0.59503 (19) | 0.02883 (12) | 0.79021 (9) | 0.0395 (5) | |
H62 | 0.5416 | 0.0482 | 0.8046 | 0.047* | |
C63 | 0.60599 (18) | 0.09786 (12) | 0.88475 (8) | 0.0375 (5) | |
C64 | 0.5843 (2) | 0.04150 (15) | 0.91118 (10) | 0.0561 (8) | |
H64 | 0.6269 | 0.0055 | 0.9107 | 0.067* | |
C65 | 0.5022 (3) | 0.0365 (2) | 0.93823 (11) | 0.0778 (12) | |
H65 | 0.4897 | −0.0024 | 0.9553 | 0.093* | |
C66 | 0.4396 (3) | 0.0885 (3) | 0.93991 (14) | 0.0893 (14) | |
H66 | 0.3841 | 0.0853 | 0.9582 | 0.107* | |
C67 | 0.4578 (3) | 0.1449 (2) | 0.91489 (14) | 0.0792 (11) | |
H67 | 0.4152 | 0.1809 | 0.9161 | 0.095* | |
C68 | 0.5396 (2) | 0.14901 (17) | 0.88768 (10) | 0.0545 (7) | |
H68 | 0.5507 | 0.1881 | 0.8705 | 0.065* | |
B1 | 0.24281 (18) | 0.35194 (13) | −0.00058 (9) | 0.0300 (5) | |
B2 | 0.7012 (2) | 0.09858 (12) | 0.85061 (9) | 0.0330 (5) | |
N1 | 0.67242 (13) | 0.38986 (10) | 0.10526 (7) | 0.0328 (4) | |
N2 | 0.60115 (13) | 0.21081 (10) | 0.08637 (6) | 0.0307 (4) | |
N3 | 0.97026 (14) | 0.17461 (10) | 0.16973 (7) | 0.0348 (4) | |
N4 | 0.68384 (16) | 0.28788 (10) | 0.29912 (7) | 0.0403 (5) | |
O1 | 0.50180 (11) | 0.36135 (9) | 0.11476 (6) | 0.0417 (4) | |
O2 | 0.57471 (12) | 0.43304 (8) | 0.17894 (6) | 0.0403 (4) | |
O3 | 0.82973 (12) | 0.39110 (9) | 0.06758 (6) | 0.0397 (4) | |
O4 | 0.82995 (12) | 0.40627 (8) | 0.15648 (6) | 0.0368 (4) | |
O5 | 0.63286 (12) | 0.13536 (8) | 0.16203 (6) | 0.0347 (3) | |
O6 | 0.47829 (11) | 0.19577 (9) | 0.14555 (6) | 0.0377 (4) | |
O7 | 0.74828 (12) | 0.15562 (9) | 0.04301 (6) | 0.0414 (4) | |
O8 | 0.68762 (12) | 0.26949 (9) | 0.02228 (5) | 0.0394 (4) | |
O9 | 0.91393 (12) | 0.26459 (9) | 0.23346 (6) | 0.0404 (4) | |
O10 | 1.03879 (11) | 0.28944 (8) | 0.17266 (6) | 0.0376 (4) | |
O11 | 0.84541 (14) | 0.08523 (8) | 0.14330 (7) | 0.0469 (4) | |
O12 | 0.95116 (12) | 0.12845 (8) | 0.08326 (6) | 0.0403 (4) | |
O13 | 0.57071 (16) | 0.39052 (10) | 0.28304 (7) | 0.0561 (5) | |
O14 | 0.73123 (15) | 0.40991 (10) | 0.27612 (8) | 0.0573 (5) | |
O15 | 0.58122 (13) | 0.18081 (10) | 0.27603 (6) | 0.0477 (4) | |
O16 | 0.75919 (13) | 0.17848 (9) | 0.27801 (6) | 0.0440 (4) | |
P1 | 0.59530 (4) | 0.36876 (3) | 0.14741 (2) | 0.02903 (12) | |
P2 | 0.78467 (4) | 0.36107 (3) | 0.11485 (2) | 0.02791 (11) | |
P3 | 0.59161 (4) | 0.20599 (3) | 0.146395 (19) | 0.02736 (11) | |
P4 | 0.71172 (4) | 0.22250 (3) | 0.066653 (19) | 0.02898 (12) | |
P5 | 0.93796 (4) | 0.25355 (3) | 0.17927 (2) | 0.02862 (12) | |
P6 | 0.89047 (4) | 0.15314 (3) | 0.12709 (2) | 0.03076 (12) | |
P7 | 0.66074 (5) | 0.35145 (3) | 0.26195 (2) | 0.03718 (14) | |
P8 | 0.67130 (4) | 0.22378 (3) | 0.26176 (2) | 0.03160 (12) | |
Rh1 | 0.646168 (12) | 0.286987 (8) | 0.195882 (6) | 0.02576 (5) | |
Rh2 | 0.814582 (11) | 0.251932 (8) | 0.125405 (5) | 0.02466 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0259 (12) | 0.0680 (19) | 0.073 (2) | −0.0019 (12) | −0.0066 (12) | 0.0170 (16) |
C2 | 0.083 (2) | 0.0412 (16) | 0.082 (2) | 0.0253 (16) | −0.0134 (19) | 0.0030 (16) |
C3 | 0.0388 (14) | 0.0533 (16) | 0.0498 (15) | −0.0079 (12) | 0.0135 (12) | 0.0038 (13) |
C4 | 0.0637 (19) | 0.0350 (14) | 0.076 (2) | −0.0052 (13) | −0.0036 (16) | −0.0118 (14) |
C5 | 0.0490 (16) | 0.0647 (19) | 0.0488 (16) | 0.0125 (14) | 0.0017 (12) | 0.0313 (14) |
C6 | 0.0674 (19) | 0.0339 (13) | 0.0552 (17) | −0.0095 (13) | −0.0021 (14) | −0.0044 (12) |
C7 | 0.0347 (14) | 0.084 (2) | 0.0417 (14) | −0.0072 (14) | 0.0085 (11) | 0.0113 (14) |
C8 | 0.0599 (18) | 0.0671 (19) | 0.0423 (15) | −0.0076 (15) | −0.0033 (13) | −0.0272 (14) |
C9 | 0.0455 (15) | 0.085 (2) | 0.0291 (12) | −0.0159 (15) | 0.0049 (11) | 0.0098 (13) |
C10 | 0.0316 (12) | 0.0676 (18) | 0.0310 (12) | −0.0106 (12) | −0.0090 (10) | 0.0037 (11) |
C11 | 0.0543 (18) | 0.100 (3) | 0.0291 (13) | −0.0045 (17) | −0.0113 (12) | 0.0064 (15) |
C12 | 0.0404 (14) | 0.0451 (15) | 0.0571 (16) | −0.0107 (12) | −0.0102 (12) | 0.0011 (12) |
C13 | 0.151 (5) | 0.0340 (19) | 0.242 (7) | −0.008 (2) | 0.117 (5) | −0.009 (3) |
C14 | 0.0403 (14) | 0.0551 (16) | 0.0396 (13) | 0.0021 (12) | 0.0082 (11) | 0.0005 (12) |
C15 | 0.0439 (15) | 0.0500 (16) | 0.0611 (18) | 0.0109 (12) | −0.0138 (13) | 0.0103 (13) |
C16 | 0.0491 (19) | 0.099 (3) | 0.074 (2) | 0.0109 (18) | 0.0175 (16) | −0.010 (2) |
C17 | 0.057 (2) | 0.079 (2) | 0.081 (2) | 0.0011 (18) | 0.0104 (18) | −0.004 (2) |
C18 | 0.105 (3) | 0.096 (3) | 0.0458 (18) | −0.048 (2) | 0.0071 (18) | 0.0117 (18) |
C19 | 0.072 (2) | 0.0608 (19) | 0.0468 (16) | 0.0240 (16) | −0.0057 (14) | −0.0008 (14) |
C20 | 0.092 (2) | 0.0608 (19) | 0.0288 (13) | −0.0076 (17) | −0.0108 (14) | −0.0013 (12) |
C21 | 0.0246 (10) | 0.0341 (12) | 0.0412 (12) | 0.0003 (9) | −0.0042 (9) | 0.0048 (10) |
C22 | 0.0395 (13) | 0.0431 (14) | 0.0389 (13) | −0.0069 (11) | −0.0046 (10) | 0.0042 (11) |
C23 | 0.0549 (17) | 0.0593 (18) | 0.0467 (16) | −0.0146 (14) | −0.0065 (13) | 0.0151 (14) |
C24 | 0.0441 (15) | 0.0505 (17) | 0.073 (2) | −0.0062 (13) | −0.0041 (14) | 0.0268 (15) |
C25 | 0.0458 (16) | 0.0352 (14) | 0.092 (2) | 0.0077 (12) | 0.0135 (15) | 0.0051 (15) |
C26 | 0.0462 (15) | 0.0381 (14) | 0.0585 (17) | 0.0048 (11) | 0.0147 (13) | 0.0035 (12) |
C27 | 0.0299 (11) | 0.0258 (10) | 0.0358 (11) | −0.0026 (8) | −0.0024 (9) | 0.0010 (9) |
C28 | 0.0353 (13) | 0.0453 (14) | 0.0398 (13) | 0.0014 (11) | −0.0026 (10) | 0.0079 (11) |
C29 | 0.0296 (12) | 0.0478 (15) | 0.0601 (17) | 0.0012 (11) | 0.0014 (11) | 0.0055 (13) |
C30 | 0.0403 (14) | 0.0476 (15) | 0.0512 (15) | −0.0062 (12) | 0.0127 (12) | −0.0029 (12) |
C31 | 0.0496 (15) | 0.0522 (15) | 0.0324 (12) | −0.0077 (12) | 0.0012 (11) | −0.0032 (11) |
C32 | 0.0320 (12) | 0.0405 (13) | 0.0348 (12) | −0.0031 (10) | −0.0046 (9) | −0.0027 (10) |
C33 | 0.0286 (11) | 0.0332 (11) | 0.0305 (11) | 0.0010 (9) | 0.0013 (9) | 0.0012 (9) |
C34 | 0.0349 (12) | 0.0324 (12) | 0.0364 (12) | 0.0008 (9) | 0.0000 (9) | −0.0023 (9) |
C35 | 0.0362 (13) | 0.0464 (14) | 0.0391 (13) | −0.0080 (11) | 0.0001 (10) | −0.0065 (11) |
C36 | 0.0293 (12) | 0.0553 (15) | 0.0370 (13) | 0.0005 (11) | −0.0038 (10) | 0.0004 (11) |
C37 | 0.0378 (13) | 0.0420 (14) | 0.0498 (15) | 0.0054 (11) | −0.0064 (11) | 0.0094 (11) |
C38 | 0.0338 (12) | 0.0338 (12) | 0.0461 (14) | −0.0014 (10) | −0.0077 (10) | 0.0061 (10) |
C39 | 0.0377 (12) | 0.0323 (12) | 0.0330 (11) | 0.0067 (10) | −0.0092 (9) | 0.0032 (9) |
C40 | 0.0405 (14) | 0.0522 (16) | 0.0491 (15) | 0.0160 (12) | −0.0088 (12) | −0.0099 (12) |
C41 | 0.065 (2) | 0.067 (2) | 0.0574 (18) | 0.0340 (17) | −0.0161 (15) | −0.0254 (16) |
C42 | 0.083 (2) | 0.0417 (16) | 0.069 (2) | 0.0198 (16) | −0.0374 (18) | −0.0208 (15) |
C43 | 0.073 (2) | 0.0353 (14) | 0.0591 (18) | −0.0048 (14) | −0.0277 (16) | 0.0028 (13) |
C44 | 0.0540 (16) | 0.0341 (12) | 0.0386 (13) | −0.0014 (11) | −0.0111 (11) | 0.0063 (10) |
C45 | 0.0294 (11) | 0.0274 (11) | 0.0417 (12) | 0.0024 (9) | −0.0067 (9) | −0.0040 (9) |
C46 | 0.0575 (17) | 0.0339 (13) | 0.0489 (15) | 0.0022 (12) | −0.0023 (13) | −0.0071 (11) |
C47 | 0.0590 (18) | 0.0275 (13) | 0.081 (2) | −0.0017 (12) | −0.0040 (16) | −0.0117 (13) |
C48 | 0.0515 (17) | 0.0390 (15) | 0.068 (2) | −0.0033 (12) | 0.0002 (14) | 0.0109 (13) |
C49 | 0.0430 (15) | 0.0476 (15) | 0.0507 (15) | −0.0021 (12) | 0.0000 (12) | 0.0082 (12) |
C50 | 0.0312 (12) | 0.0355 (12) | 0.0416 (13) | 0.0003 (10) | −0.0046 (10) | −0.0004 (10) |
C51 | 0.0404 (13) | 0.0301 (11) | 0.0395 (13) | 0.0066 (10) | −0.0026 (10) | −0.0047 (10) |
C52 | 0.0461 (14) | 0.0384 (13) | 0.0350 (12) | 0.0028 (11) | −0.0054 (10) | −0.0028 (10) |
C53 | 0.0478 (16) | 0.0603 (18) | 0.0469 (15) | 0.0001 (13) | −0.0120 (12) | −0.0069 (13) |
C54 | 0.0567 (18) | 0.065 (2) | 0.0595 (18) | 0.0208 (16) | −0.0207 (15) | −0.0059 (15) |
C55 | 0.080 (2) | 0.0418 (16) | 0.092 (3) | 0.0226 (16) | −0.030 (2) | 0.0047 (16) |
C56 | 0.067 (2) | 0.0310 (14) | 0.091 (2) | 0.0065 (13) | −0.0281 (18) | 0.0005 (14) |
C57 | 0.0452 (13) | 0.0230 (10) | 0.0385 (12) | −0.0018 (9) | 0.0003 (10) | −0.0013 (9) |
C58 | 0.0469 (15) | 0.0370 (14) | 0.0661 (18) | −0.0038 (12) | 0.0057 (13) | −0.0166 (13) |
C59 | 0.070 (2) | 0.0399 (15) | 0.0664 (19) | 0.0002 (14) | 0.0145 (16) | −0.0204 (14) |
C60 | 0.085 (2) | 0.0347 (14) | 0.0423 (15) | −0.0024 (14) | −0.0027 (14) | −0.0098 (11) |
C61 | 0.0627 (18) | 0.0404 (14) | 0.0444 (15) | −0.0030 (13) | −0.0155 (13) | −0.0044 (12) |
C62 | 0.0482 (14) | 0.0328 (12) | 0.0375 (13) | 0.0007 (10) | −0.0048 (11) | −0.0025 (10) |
C63 | 0.0410 (13) | 0.0413 (13) | 0.0300 (11) | −0.0041 (10) | −0.0050 (10) | −0.0069 (10) |
C64 | 0.075 (2) | 0.0494 (16) | 0.0439 (15) | −0.0173 (15) | 0.0050 (14) | −0.0066 (13) |
C65 | 0.111 (3) | 0.079 (2) | 0.0432 (17) | −0.050 (2) | 0.0201 (19) | −0.0165 (17) |
C66 | 0.076 (3) | 0.123 (4) | 0.070 (2) | −0.040 (3) | 0.039 (2) | −0.044 (2) |
C67 | 0.057 (2) | 0.103 (3) | 0.078 (2) | 0.002 (2) | 0.0220 (18) | −0.023 (2) |
C68 | 0.0489 (16) | 0.0652 (19) | 0.0495 (16) | 0.0090 (14) | 0.0070 (13) | −0.0050 (14) |
B1 | 0.0272 (12) | 0.0305 (12) | 0.0322 (12) | 0.0015 (10) | −0.0023 (10) | 0.0025 (10) |
B2 | 0.0392 (14) | 0.0245 (12) | 0.0353 (13) | 0.0009 (10) | −0.0031 (11) | −0.0042 (10) |
N1 | 0.0300 (10) | 0.0368 (10) | 0.0317 (10) | 0.0046 (8) | 0.0008 (8) | 0.0115 (8) |
N2 | 0.0252 (9) | 0.0425 (11) | 0.0242 (9) | −0.0060 (8) | −0.0041 (7) | 0.0021 (8) |
N3 | 0.0341 (10) | 0.0339 (10) | 0.0362 (10) | 0.0048 (8) | −0.0068 (8) | 0.0033 (8) |
N4 | 0.0523 (13) | 0.0426 (12) | 0.0258 (10) | −0.0027 (10) | −0.0052 (9) | −0.0012 (8) |
O1 | 0.0283 (8) | 0.0526 (11) | 0.0440 (10) | 0.0002 (7) | −0.0097 (7) | 0.0091 (8) |
O2 | 0.0409 (9) | 0.0358 (9) | 0.0442 (10) | 0.0107 (7) | −0.0008 (7) | 0.0015 (7) |
O3 | 0.0378 (9) | 0.0430 (9) | 0.0385 (9) | −0.0017 (7) | 0.0091 (7) | 0.0099 (7) |
O4 | 0.0368 (9) | 0.0319 (8) | 0.0416 (9) | −0.0025 (7) | −0.0035 (7) | −0.0037 (7) |
O5 | 0.0415 (9) | 0.0281 (8) | 0.0343 (8) | −0.0012 (7) | −0.0034 (7) | 0.0022 (6) |
O6 | 0.0264 (8) | 0.0526 (10) | 0.0339 (8) | −0.0064 (7) | 0.0006 (6) | 0.0073 (7) |
O7 | 0.0408 (9) | 0.0499 (10) | 0.0332 (9) | 0.0004 (8) | −0.0045 (7) | −0.0155 (8) |
O8 | 0.0335 (9) | 0.0595 (11) | 0.0252 (8) | −0.0064 (8) | −0.0018 (6) | 0.0103 (7) |
O9 | 0.0372 (9) | 0.0585 (11) | 0.0256 (8) | −0.0021 (8) | −0.0029 (7) | −0.0023 (7) |
O10 | 0.0292 (8) | 0.0429 (9) | 0.0406 (9) | −0.0055 (7) | −0.0008 (7) | −0.0015 (7) |
O11 | 0.0582 (12) | 0.0283 (9) | 0.0544 (11) | −0.0049 (8) | 0.0111 (9) | 0.0007 (8) |
O12 | 0.0431 (10) | 0.0369 (9) | 0.0409 (9) | 0.0072 (7) | 0.0061 (7) | −0.0041 (7) |
O13 | 0.0759 (14) | 0.0476 (11) | 0.0449 (11) | 0.0093 (10) | 0.0038 (10) | −0.0114 (9) |
O14 | 0.0572 (13) | 0.0532 (12) | 0.0613 (13) | −0.0093 (10) | −0.0086 (10) | −0.0068 (10) |
O15 | 0.0507 (11) | 0.0552 (11) | 0.0374 (9) | −0.0162 (9) | 0.0042 (8) | 0.0054 (8) |
O16 | 0.0466 (10) | 0.0440 (10) | 0.0412 (9) | 0.0066 (8) | −0.0095 (8) | 0.0080 (8) |
P1 | 0.0242 (3) | 0.0319 (3) | 0.0309 (3) | 0.0019 (2) | −0.0022 (2) | 0.0055 (2) |
P2 | 0.0263 (3) | 0.0294 (3) | 0.0280 (3) | −0.0007 (2) | 0.0003 (2) | 0.0037 (2) |
P3 | 0.0255 (3) | 0.0318 (3) | 0.0248 (3) | −0.0023 (2) | −0.0012 (2) | 0.0031 (2) |
P4 | 0.0265 (3) | 0.0383 (3) | 0.0221 (3) | −0.0034 (2) | −0.0018 (2) | −0.0008 (2) |
P5 | 0.0267 (3) | 0.0336 (3) | 0.0255 (3) | −0.0011 (2) | −0.0032 (2) | −0.0003 (2) |
P6 | 0.0321 (3) | 0.0280 (3) | 0.0321 (3) | 0.0009 (2) | −0.0001 (2) | −0.0010 (2) |
P7 | 0.0462 (4) | 0.0346 (3) | 0.0306 (3) | −0.0046 (3) | −0.0035 (3) | −0.0023 (2) |
P8 | 0.0356 (3) | 0.0351 (3) | 0.0241 (3) | −0.0014 (2) | −0.0025 (2) | 0.0041 (2) |
Rh1 | 0.02586 (8) | 0.02892 (9) | 0.02246 (8) | 0.00076 (6) | −0.00106 (6) | 0.00267 (6) |
Rh2 | 0.02377 (8) | 0.02735 (9) | 0.02277 (8) | −0.00055 (6) | −0.00253 (6) | −0.00053 (6) |
C1—O1 | 1.449 (3) | C51—C56 | 1.399 (4) |
C2—O2 | 1.439 (3) | C51—B2 | 1.652 (4) |
C3—O3 | 1.446 (3) | C52—C53 | 1.385 (4) |
C4—O4 | 1.443 (3) | C53—C54 | 1.374 (4) |
C5—N1 | 1.491 (3) | C54—C55 | 1.366 (5) |
C6—O5 | 1.444 (3) | C55—C56 | 1.390 (4) |
C7—O6 | 1.434 (3) | C57—C62 | 1.394 (3) |
C8—O7 | 1.454 (3) | C57—C58 | 1.400 (4) |
C9—O8 | 1.447 (3) | C57—B2 | 1.646 (3) |
C10—N2 | 1.491 (3) | C58—C59 | 1.388 (4) |
C11—O9 | 1.450 (3) | C59—C60 | 1.384 (4) |
C12—O10 | 1.439 (3) | C60—C61 | 1.376 (4) |
C13—O11 | 1.387 (4) | C61—C62 | 1.393 (3) |
C14—O12 | 1.441 (3) | C63—C68 | 1.392 (4) |
C15—N3 | 1.474 (3) | C63—C64 | 1.396 (4) |
C16—O13 | 1.446 (4) | C63—B2 | 1.653 (4) |
C17—O14 | 1.385 (4) | C64—C65 | 1.391 (5) |
C18—O15 | 1.405 (3) | C65—C66 | 1.368 (6) |
C19—O16 | 1.434 (3) | C66—C67 | 1.367 (6) |
C20—N4 | 1.474 (3) | C67—C68 | 1.388 (4) |
C21—C26 | 1.396 (4) | N1—P1 | 1.6700 (19) |
C21—C22 | 1.396 (3) | N1—P2 | 1.6914 (19) |
C21—B1 | 1.654 (3) | N2—P4 | 1.6665 (19) |
C22—C23 | 1.386 (4) | N2—P3 | 1.6995 (18) |
C23—C24 | 1.351 (4) | N3—P5 | 1.680 (2) |
C24—C25 | 1.369 (5) | N3—P6 | 1.683 (2) |
C25—C26 | 1.403 (4) | N4—P8 | 1.676 (2) |
C27—C32 | 1.385 (3) | N4—P7 | 1.685 (2) |
C27—C28 | 1.407 (3) | O1—P1 | 1.5938 (17) |
C27—B1 | 1.641 (3) | O2—P1 | 1.6014 (18) |
C28—C29 | 1.385 (4) | O3—P2 | 1.5999 (16) |
C29—C30 | 1.376 (4) | O4—P2 | 1.6082 (17) |
C30—C31 | 1.375 (4) | O5—P3 | 1.5985 (16) |
C31—C32 | 1.393 (3) | O6—P3 | 1.5972 (16) |
C33—C38 | 1.401 (3) | O7—P4 | 1.5937 (18) |
C33—C34 | 1.401 (3) | O8—P4 | 1.6007 (17) |
C33—B1 | 1.648 (3) | O9—P5 | 1.5825 (17) |
C34—C35 | 1.394 (3) | O10—P5 | 1.5984 (17) |
C35—C36 | 1.374 (4) | O11—P6 | 1.5799 (18) |
C36—C37 | 1.378 (4) | O12—P6 | 1.5877 (17) |
C37—C38 | 1.388 (3) | O13—P7 | 1.607 (2) |
C39—C44 | 1.396 (4) | O14—P7 | 1.586 (2) |
C39—C40 | 1.403 (4) | O15—P8 | 1.5860 (18) |
C39—B1 | 1.652 (3) | O16—P8 | 1.5935 (18) |
C40—C41 | 1.389 (4) | P1—Rh1 | 2.2512 (6) |
C41—C42 | 1.369 (5) | P2—Rh2 | 2.2631 (6) |
C42—C43 | 1.374 (5) | P3—Rh1 | 2.2736 (6) |
C43—C44 | 1.392 (4) | P4—Rh2 | 2.2552 (6) |
C45—C50 | 1.397 (3) | P5—Rh2 | 2.2796 (6) |
C45—C46 | 1.404 (3) | P5—P6 | 2.5853 (8) |
C45—B2 | 1.643 (3) | P6—Rh2 | 2.2606 (6) |
C46—C47 | 1.399 (4) | P7—Rh1 | 2.2769 (6) |
C47—C48 | 1.372 (5) | P7—P8 | 2.5837 (9) |
C48—C49 | 1.365 (4) | P8—Rh1 | 2.2746 (6) |
C49—C50 | 1.386 (4) | Rh1—Rh2 | 3.1805 (2) |
C51—C52 | 1.392 (3) | ||
C26—C21—C22 | 114.6 (2) | C6—O5—P3 | 121.56 (16) |
C26—C21—B1 | 121.5 (2) | C7—O6—P3 | 120.49 (16) |
C22—C21—B1 | 123.9 (2) | C8—O7—P4 | 126.03 (18) |
C23—C22—C21 | 123.1 (3) | C9—O8—P4 | 119.08 (17) |
C24—C23—C22 | 120.5 (3) | C11—O9—P5 | 123.94 (18) |
C23—C24—C25 | 119.5 (3) | C12—O10—P5 | 121.29 (16) |
C24—C25—C26 | 120.0 (3) | C13—O11—P6 | 129.0 (2) |
C21—C26—C25 | 122.3 (3) | C14—O12—P6 | 119.90 (15) |
C32—C27—C28 | 115.1 (2) | C16—O13—P7 | 119.45 (19) |
C32—C27—B1 | 125.0 (2) | C17—O14—P7 | 120.5 (2) |
C28—C27—B1 | 119.8 (2) | C18—O15—P8 | 126.0 (2) |
C29—C28—C27 | 122.6 (2) | C19—O16—P8 | 119.29 (17) |
C30—C29—C28 | 120.2 (2) | O1—P1—O2 | 104.07 (10) |
C31—C30—C29 | 118.9 (2) | O1—P1—N1 | 98.44 (9) |
C30—C31—C32 | 120.4 (2) | O2—P1—N1 | 108.05 (10) |
C27—C32—C31 | 122.7 (2) | O1—P1—Rh1 | 121.98 (7) |
C38—C33—C34 | 114.8 (2) | O2—P1—Rh1 | 108.49 (7) |
C38—C33—B1 | 122.2 (2) | N1—P1—Rh1 | 114.61 (7) |
C34—C33—B1 | 123.0 (2) | O3—P2—O4 | 103.59 (9) |
C35—C34—C33 | 122.6 (2) | O3—P2—N1 | 96.46 (9) |
C36—C35—C34 | 120.6 (2) | O4—P2—N1 | 105.97 (10) |
C35—C36—C37 | 118.6 (2) | O3—P2—Rh2 | 113.86 (7) |
C36—C37—C38 | 120.6 (2) | O4—P2—Rh2 | 112.81 (7) |
C37—C38—C33 | 122.9 (2) | N1—P2—Rh2 | 121.69 (7) |
C44—C39—C40 | 114.7 (2) | O6—P3—O5 | 104.03 (9) |
C44—C39—B1 | 124.2 (2) | O6—P3—N2 | 94.88 (9) |
C40—C39—B1 | 121.1 (2) | O5—P3—N2 | 106.95 (9) |
C41—C40—C39 | 122.6 (3) | O6—P3—Rh1 | 115.20 (7) |
C42—C41—C40 | 120.3 (3) | O5—P3—Rh1 | 110.95 (6) |
C41—C42—C43 | 119.4 (3) | N2—P3—Rh1 | 122.49 (7) |
C42—C43—C44 | 119.9 (3) | O7—P4—O8 | 104.03 (10) |
C43—C44—C39 | 123.0 (3) | O7—P4—N2 | 108.87 (10) |
C50—C45—C46 | 114.2 (2) | O8—P4—N2 | 99.11 (9) |
C50—C45—B2 | 122.5 (2) | O7—P4—Rh2 | 108.95 (7) |
C46—C45—B2 | 123.3 (2) | O8—P4—Rh2 | 122.70 (7) |
C47—C46—C45 | 122.3 (3) | N2—P4—Rh2 | 112.18 (7) |
C48—C47—C46 | 120.5 (3) | O9—P5—O10 | 104.37 (9) |
C49—C48—C47 | 119.1 (3) | O9—P5—N3 | 110.44 (10) |
C48—C49—C50 | 120.1 (3) | O10—P5—N3 | 99.95 (10) |
C49—C50—C45 | 123.8 (2) | O9—P5—Rh2 | 118.28 (7) |
C52—C51—C56 | 113.8 (2) | O10—P5—Rh2 | 126.08 (7) |
C52—C51—B2 | 124.9 (2) | N3—P5—Rh2 | 94.74 (7) |
C56—C51—B2 | 121.4 (2) | O9—P5—P6 | 127.00 (7) |
C53—C52—C51 | 123.3 (3) | O10—P5—P6 | 120.63 (7) |
C54—C53—C52 | 120.8 (3) | Rh2—P5—P6 | 54.942 (18) |
C55—C54—C53 | 118.4 (3) | O11—P6—O12 | 99.86 (10) |
C54—C55—C56 | 120.3 (3) | O11—P6—N3 | 106.30 (10) |
C55—C56—C51 | 123.5 (3) | O12—P6—N3 | 106.20 (10) |
C62—C57—C58 | 115.5 (2) | O11—P6—Rh2 | 125.73 (8) |
C62—C57—B2 | 120.8 (2) | O12—P6—Rh2 | 121.14 (7) |
C58—C57—B2 | 123.1 (2) | N3—P6—Rh2 | 95.35 (7) |
C59—C58—C57 | 122.1 (3) | O11—P6—P5 | 128.14 (8) |
C60—C59—C58 | 120.7 (3) | O12—P6—P5 | 123.52 (7) |
C61—C60—C59 | 118.7 (3) | Rh2—P6—P5 | 55.638 (18) |
C60—C61—C62 | 120.1 (3) | O14—P7—O13 | 91.62 (12) |
C61—C62—C57 | 122.8 (3) | O14—P7—N4 | 107.40 (11) |
C68—C63—C64 | 115.1 (3) | O13—P7—N4 | 106.80 (11) |
C68—C63—B2 | 124.8 (2) | O14—P7—Rh1 | 132.80 (9) |
C64—C63—B2 | 120.0 (2) | O13—P7—Rh1 | 121.45 (8) |
C65—C64—C63 | 122.5 (3) | N4—P7—Rh1 | 94.88 (7) |
C66—C65—C64 | 119.8 (4) | O14—P7—P8 | 135.15 (9) |
C67—C66—C65 | 119.9 (3) | O13—P7—P8 | 122.44 (8) |
C66—C67—C68 | 119.7 (4) | Rh1—P7—P8 | 55.370 (19) |
C67—C68—C63 | 122.9 (3) | O15—P8—O16 | 102.97 (10) |
C27—B1—C33 | 110.34 (18) | O15—P8—N4 | 109.89 (11) |
C27—B1—C39 | 109.32 (18) | O16—P8—N4 | 100.99 (10) |
C33—B1—C39 | 109.23 (18) | O15—P8—Rh1 | 113.58 (7) |
C27—B1—C21 | 108.05 (18) | O16—P8—Rh1 | 131.73 (7) |
C33—B1—C21 | 108.78 (18) | N4—P8—Rh1 | 95.22 (7) |
C39—B1—C21 | 111.11 (18) | O15—P8—P7 | 120.02 (8) |
C45—B2—C57 | 107.09 (19) | O16—P8—P7 | 128.07 (8) |
C45—B2—C51 | 109.02 (19) | Rh1—P8—P7 | 55.454 (19) |
C57—B2—C51 | 111.15 (19) | P1—Rh1—P3 | 93.26 (2) |
C45—B2—C63 | 112.56 (19) | P1—Rh1—P8 | 161.76 (2) |
C57—B2—C63 | 107.61 (19) | P3—Rh1—P8 | 98.15 (2) |
C51—B2—C63 | 109.42 (19) | P1—Rh1—P7 | 95.67 (2) |
C5—N1—P1 | 122.72 (16) | P3—Rh1—P7 | 159.60 (2) |
C5—N1—P2 | 123.33 (16) | P8—Rh1—P7 | 69.18 (2) |
P1—N1—P2 | 113.94 (10) | P1—Rh1—Rh2 | 90.891 (16) |
C10—N2—P4 | 122.36 (15) | P3—Rh1—Rh2 | 72.681 (15) |
C10—N2—P3 | 122.25 (15) | P8—Rh1—Rh2 | 106.054 (17) |
P4—N2—P3 | 115.21 (10) | P7—Rh1—Rh2 | 125.352 (19) |
C15—N3—P5 | 131.17 (18) | P4—Rh2—P6 | 94.39 (2) |
C15—N3—P6 | 127.50 (18) | P4—Rh2—P2 | 92.64 (2) |
P5—N3—P6 | 100.47 (10) | P6—Rh2—P2 | 161.59 (2) |
C20—N4—P8 | 131.63 (19) | P4—Rh2—P5 | 163.61 (2) |
C20—N4—P7 | 127.53 (19) | P6—Rh2—P5 | 69.42 (2) |
P8—N4—P7 | 100.50 (11) | P2—Rh2—P5 | 102.12 (2) |
C1—O1—P1 | 119.84 (17) | P4—Rh2—Rh1 | 92.651 (15) |
C2—O2—P1 | 124.63 (19) | P6—Rh2—Rh1 | 122.341 (16) |
C3—O3—P2 | 118.31 (16) | P2—Rh2—Rh1 | 74.210 (15) |
C4—O4—P2 | 121.02 (17) | P5—Rh2—Rh1 | 98.148 (16) |
Experimental details
Crystal data | |
Chemical formula | C20H60N4O16P8Rh2·2(C24H20B) |
Mr | 1704.72 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 225 |
a, b, c (Å) | 13.9783 (3), 20.2046 (5), 28.1465 (7) |
β (°) | 90.842 (1) |
V (Å3) | 7948.4 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.64 |
Crystal size (mm) | 0.31 × 0.18 × 0.10 |
Data collection | |
Diffractometer | Bruker APEX-II CCD diffractometer |
Absorption correction | Numerical BRUKER SADABS |
Tmin, Tmax | 0.826, 0.939 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 17345, 17345, 14691 |
Rint | 0.000 |
(sin θ/λ)max (Å−1) | 0.639 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.030, 0.081, 1.03 |
No. of reflections | 17345 |
No. of parameters | 905 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.12, −0.40 |
Computer programs: Bruker APEX2, Bruker SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL.