Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804013662/na6341sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804013662/na6341Isup2.hkl |
CCDC reference: 245138
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[Cd(C22H12O6)(C10H8N2)(H2O)2](C3H7NO) | F(000) = 1528 |
Mr = 750.03 | Dx = 1.480 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 14.376 (6) Å | Cell parameters from 3369 reflections |
b = 20.576 (8) Å | θ = 5–28° |
c = 11.383 (4) Å | µ = 0.71 mm−1 |
β = 90.301 (7)° | T = 293 K |
V = 3367 (2) Å3 | BLOCK, yellow |
Z = 4 | 0.28 × 0.22 × 0.16 mm |
Bruker SMART CCD area-detector diffractometer | 7134 independent reflections |
Radiation source: fine-focus sealed tube | 3369 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.067 |
φ and ω scans | θmax = 27.0°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −18→18 |
Tmin = 0.827, Tmax = 0.895 | k = −26→18 |
19183 measured reflections | l = −13→14 |
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)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.084 | H-atom parameters constrained |
S = 0.96 | w = 1/[σ2(Fo2) + (0.020P)2] where P = (Fo2 + 2Fc2)/3 |
7134 reflections | (Δ/σ)max = 0.002 |
433 parameters | Δρmax = 0.63 e Å−3 |
0 restraints | Δρmin = −0.54 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 | ||
Cd1 | 0.40490 (2) | 0.669119 (15) | 0.00034 (3) | 0.05446 (12) | |
O1W | 0.3660 (2) | 0.70547 (15) | −0.1927 (3) | 0.0763 (10) | |
H1WA | 0.4114 | 0.7160 | −0.2381 | 0.092* | |
H1WB | 0.3199 | 0.7316 | −0.1998 | 0.092* | |
O2W | 0.2763 (2) | 0.71868 (16) | 0.0678 (3) | 0.0853 (10) | |
H2WA | 0.2295 | 0.6922 | 0.0698 | 0.102* | |
H2WB | 0.2589 | 0.7500 | 0.0209 | 0.102* | |
O1 | 0.5499 (2) | 0.70339 (14) | −0.0542 (3) | 0.0660 (9) | |
O2 | 0.5190 (2) | 0.75984 (14) | 0.1108 (3) | 0.0715 (10) | |
O3 | 0.62448 (19) | 0.85563 (13) | 0.1744 (3) | 0.0654 (9) | |
H3A | 0.5784 | 0.8300 | 0.1896 | 0.078* | |
O4 | 0.7463 (2) | 1.18461 (13) | 0.1698 (3) | 0.0652 (9) | |
O5 | 0.7031 (2) | 1.13819 (13) | −0.0025 (3) | 0.0720 (9) | |
O6 | 0.70460 (19) | 1.01475 (12) | −0.0250 (2) | 0.0590 (8) | |
H6B | 0.6890 | 1.0525 | −0.0528 | 0.071* | |
N1 | 0.3643 (2) | 0.56138 (16) | −0.0496 (3) | 0.0515 (9) | |
N2 | 0.4464 (2) | 0.60081 (16) | 0.1579 (3) | 0.0458 (9) | |
C1 | 0.7503 (3) | 0.88781 (17) | 0.0507 (3) | 0.0387 (10) | |
C2 | 0.6768 (3) | 0.84524 (18) | 0.0759 (4) | 0.0445 (11) | |
C3 | 0.6541 (3) | 0.79049 (19) | −0.0015 (4) | 0.0450 (11) | |
C4 | 0.7103 (3) | 0.78047 (19) | −0.0984 (4) | 0.0554 (12) | |
H4A | 0.6951 | 0.7438 | −0.1525 | 0.066* | |
C5 | 0.8468 (4) | 0.8094 (2) | −0.2255 (4) | 0.0726 (15) | |
H5A | 0.8326 | 0.7729 | −0.2805 | 0.087* | |
C6 | 0.9241 (4) | 0.8478 (2) | −0.2473 (4) | 0.0788 (16) | |
H6A | 0.9637 | 0.8385 | −0.3151 | 0.095* | |
C7 | 0.9433 (3) | 0.9020 (2) | −0.1717 (5) | 0.0691 (14) | |
H7A | 0.9964 | 0.9297 | −0.1893 | 0.083* | |
C8 | 0.8878 (3) | 0.9152 (2) | −0.0767 (4) | 0.0517 (11) | |
H8A | 0.9032 | 0.9530 | −0.0252 | 0.062* | |
C9 | 0.8081 (3) | 0.87554 (19) | −0.0495 (3) | 0.0421 (10) | |
C10 | 0.7890 (3) | 0.8209 (2) | −0.1248 (4) | 0.0493 (11) | |
C11 | 0.7674 (2) | 0.94815 (18) | 0.1271 (3) | 0.0387 (10) | |
C12 | 0.7451 (3) | 1.01002 (19) | 0.0837 (4) | 0.0409 (10) | |
C13 | 0.7619 (3) | 1.06866 (18) | 0.1514 (3) | 0.0395 (10) | |
C14 | 0.8045 (3) | 1.06264 (19) | 0.2613 (4) | 0.0439 (11) | |
H14A | 0.8162 | 1.1012 | 0.3070 | 0.053* | |
C15 | 0.8748 (3) | 0.9957 (2) | 0.4224 (4) | 0.0564 (12) | |
H15A | 0.8874 | 1.0357 | 0.4667 | 0.068* | |
C16 | 0.8990 (3) | 0.9357 (3) | 0.4686 (4) | 0.0653 (14) | |
H16A | 0.9308 | 0.9333 | 0.5450 | 0.078* | |
C17 | 0.8794 (3) | 0.8778 (2) | 0.4031 (5) | 0.0670 (14) | |
H17A | 0.8971 | 0.8351 | 0.4356 | 0.080* | |
C18 | 0.8362 (3) | 0.88117 (19) | 0.2931 (4) | 0.0528 (12) | |
H18A | 0.8224 | 0.8411 | 0.2492 | 0.063* | |
C19 | 0.8106 (3) | 0.94275 (19) | 0.2422 (4) | 0.0425 (10) | |
C20 | 0.8298 (3) | 1.0007 (2) | 0.3093 (4) | 0.0434 (10) | |
C21 | 0.5698 (3) | 0.7484 (2) | 0.0195 (5) | 0.0574 (13) | |
C22 | 0.7355 (3) | 1.1353 (2) | 0.1030 (4) | 0.0508 (11) | |
C23 | 0.3213 (3) | 0.5452 (3) | −0.1526 (4) | 0.0707 (14) | |
H23A | 0.3064 | 0.5800 | −0.2113 | 0.085* | |
C24 | 0.2979 (3) | 0.4811 (3) | −0.1785 (4) | 0.0774 (16) | |
H24A | 0.2679 | 0.4710 | −0.2548 | 0.093* | |
C25 | 0.3159 (3) | 0.4325 (2) | −0.0966 (5) | 0.0703 (15) | |
H25A | 0.2999 | 0.3872 | −0.1143 | 0.084* | |
C26 | 0.3591 (3) | 0.4490 (2) | 0.0096 (4) | 0.0507 (12) | |
H26A | 0.3729 | 0.4148 | 0.0691 | 0.061* | |
C27 | 0.3814 (3) | 0.51470 (19) | 0.0322 (4) | 0.0417 (10) | |
C28 | 0.4278 (3) | 0.53585 (19) | 0.1456 (3) | 0.0406 (10) | |
C29 | 0.4506 (3) | 0.4913 (2) | 0.2341 (4) | 0.0532 (12) | |
H29A | 0.4372 | 0.4446 | 0.2235 | 0.064* | |
C30 | 0.4932 (3) | 0.5135 (2) | 0.3373 (4) | 0.0665 (14) | |
H30A | 0.5097 | 0.4829 | 0.4003 | 0.080* | |
C31 | 0.5115 (3) | 0.5796 (2) | 0.3511 (4) | 0.0658 (14) | |
H31A | 0.5426 | 0.5963 | 0.4220 | 0.079* | |
C32 | 0.4872 (3) | 0.6215 (2) | 0.2598 (4) | 0.0586 (12) | |
H32A | 0.4973 | 0.6684 | 0.2698 | 0.070* | |
O7 | 0.1286 (3) | 0.6569 (2) | 0.9123 (4) | 0.1240 (16) | |
N3 | 0.0822 (3) | 0.6557 (2) | 0.7174 (4) | 0.0792 (12) | |
C33 | 0.0814 (4) | 0.5843 (3) | 0.7077 (6) | 0.109 (2) | |
H33A | 0.1015 | 0.5648 | 0.7803 | 0.163* | |
H33B | 0.0187 | 0.5688 | 0.6903 | 0.163* | |
H33C | 0.1215 | 0.5698 | 0.6453 | 0.163* | |
C34 | 0.0532 (4) | 0.6923 (3) | 0.6134 (5) | 0.0994 (19) | |
H34A | 0.0556 | 0.7388 | 0.6280 | 0.149* | |
H34B | 0.0917 | 0.6831 | 0.5462 | 0.149* | |
H34C | −0.0112 | 0.6820 | 0.5912 | 0.149* | |
C35 | 0.1067 (4) | 0.6848 (3) | 0.8187 (7) | 0.0945 (19) | |
H35A | 0.1065 | 0.7333 | 0.8165 | 0.113* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0625 (2) | 0.04106 (18) | 0.0598 (2) | 0.0006 (2) | −0.00569 (15) | 0.0094 (2) |
O1W | 0.078 (2) | 0.080 (2) | 0.071 (2) | 0.0123 (19) | 0.0008 (18) | 0.0262 (19) |
O2W | 0.094 (2) | 0.076 (2) | 0.086 (2) | −0.005 (2) | −0.011 (2) | 0.016 (2) |
O1 | 0.081 (2) | 0.0392 (18) | 0.078 (2) | −0.0129 (17) | −0.0144 (18) | −0.0101 (18) |
O2 | 0.063 (2) | 0.047 (2) | 0.105 (3) | −0.0196 (17) | 0.009 (2) | −0.0020 (19) |
O3 | 0.069 (2) | 0.0484 (19) | 0.079 (2) | −0.0151 (16) | 0.0293 (19) | −0.0111 (17) |
O4 | 0.094 (2) | 0.0346 (19) | 0.067 (2) | 0.0038 (16) | 0.0049 (18) | −0.0055 (16) |
O5 | 0.106 (3) | 0.0420 (18) | 0.068 (2) | 0.0032 (18) | −0.020 (2) | 0.0104 (17) |
O6 | 0.082 (2) | 0.0412 (17) | 0.054 (2) | 0.0049 (16) | −0.0157 (17) | 0.0035 (15) |
N1 | 0.055 (2) | 0.051 (2) | 0.048 (2) | 0.0033 (19) | −0.0048 (19) | 0.000 (2) |
N2 | 0.051 (2) | 0.040 (2) | 0.046 (2) | −0.0027 (18) | −0.0040 (18) | 0.0018 (18) |
C1 | 0.042 (2) | 0.029 (2) | 0.046 (3) | −0.001 (2) | −0.001 (2) | 0.001 (2) |
C2 | 0.046 (3) | 0.035 (3) | 0.053 (3) | 0.007 (2) | 0.007 (2) | −0.001 (2) |
C3 | 0.054 (3) | 0.027 (2) | 0.054 (3) | 0.001 (2) | 0.004 (2) | 0.003 (2) |
C4 | 0.074 (3) | 0.030 (3) | 0.062 (3) | 0.003 (2) | −0.011 (3) | −0.005 (2) |
C5 | 0.112 (4) | 0.042 (3) | 0.065 (4) | 0.012 (3) | 0.020 (3) | −0.001 (3) |
C6 | 0.105 (4) | 0.052 (3) | 0.080 (4) | 0.021 (3) | 0.039 (3) | 0.011 (3) |
C7 | 0.068 (3) | 0.054 (3) | 0.086 (4) | 0.006 (3) | 0.026 (3) | 0.018 (3) |
C8 | 0.052 (3) | 0.045 (3) | 0.059 (3) | 0.003 (2) | 0.004 (2) | 0.008 (2) |
C9 | 0.052 (3) | 0.031 (2) | 0.043 (3) | 0.003 (2) | −0.003 (2) | 0.003 (2) |
C10 | 0.063 (3) | 0.034 (3) | 0.051 (3) | 0.006 (2) | 0.009 (2) | 0.002 (2) |
C11 | 0.038 (2) | 0.033 (2) | 0.044 (3) | −0.003 (2) | 0.002 (2) | −0.001 (2) |
C12 | 0.044 (3) | 0.036 (2) | 0.043 (3) | −0.005 (2) | −0.004 (2) | −0.001 (2) |
C13 | 0.043 (2) | 0.033 (2) | 0.043 (3) | −0.002 (2) | 0.004 (2) | 0.002 (2) |
C14 | 0.043 (2) | 0.036 (2) | 0.053 (3) | −0.009 (2) | 0.005 (2) | −0.007 (2) |
C15 | 0.058 (3) | 0.058 (3) | 0.053 (3) | −0.010 (3) | −0.007 (2) | −0.005 (3) |
C16 | 0.068 (3) | 0.071 (4) | 0.057 (3) | −0.004 (3) | −0.022 (3) | 0.014 (3) |
C17 | 0.067 (3) | 0.056 (3) | 0.078 (4) | 0.003 (3) | −0.010 (3) | 0.021 (3) |
C18 | 0.057 (3) | 0.041 (3) | 0.060 (3) | −0.003 (2) | −0.006 (2) | 0.006 (2) |
C19 | 0.043 (2) | 0.036 (3) | 0.048 (3) | −0.003 (2) | 0.002 (2) | 0.008 (2) |
C20 | 0.040 (2) | 0.043 (3) | 0.047 (3) | −0.010 (2) | −0.003 (2) | 0.003 (2) |
C21 | 0.064 (4) | 0.037 (3) | 0.071 (4) | 0.005 (3) | −0.006 (3) | 0.014 (3) |
C22 | 0.055 (3) | 0.036 (3) | 0.061 (3) | 0.000 (2) | 0.007 (3) | 0.003 (3) |
C23 | 0.082 (4) | 0.078 (4) | 0.052 (3) | 0.003 (3) | −0.016 (3) | −0.002 (3) |
C24 | 0.068 (4) | 0.100 (5) | 0.064 (4) | −0.007 (3) | −0.014 (3) | −0.027 (4) |
C25 | 0.061 (3) | 0.063 (3) | 0.087 (4) | −0.012 (3) | −0.002 (3) | −0.027 (3) |
C26 | 0.057 (3) | 0.043 (3) | 0.052 (3) | −0.004 (2) | −0.003 (2) | −0.001 (2) |
C27 | 0.038 (3) | 0.040 (3) | 0.048 (3) | 0.004 (2) | 0.004 (2) | −0.002 (2) |
C28 | 0.041 (2) | 0.035 (2) | 0.045 (3) | 0.002 (2) | 0.006 (2) | 0.004 (2) |
C29 | 0.065 (3) | 0.043 (3) | 0.052 (3) | −0.006 (2) | −0.003 (3) | 0.008 (2) |
C30 | 0.082 (4) | 0.066 (4) | 0.052 (3) | 0.003 (3) | −0.005 (3) | 0.019 (3) |
C31 | 0.087 (4) | 0.067 (4) | 0.043 (3) | −0.010 (3) | −0.017 (3) | 0.003 (3) |
C32 | 0.076 (3) | 0.046 (3) | 0.053 (3) | −0.005 (3) | −0.005 (3) | −0.007 (3) |
O7 | 0.123 (3) | 0.121 (4) | 0.127 (4) | −0.027 (3) | −0.058 (3) | 0.003 (3) |
N3 | 0.062 (3) | 0.068 (3) | 0.108 (4) | −0.007 (2) | −0.009 (3) | −0.014 (3) |
C33 | 0.103 (4) | 0.070 (4) | 0.153 (6) | 0.003 (4) | −0.008 (4) | −0.028 (4) |
C34 | 0.105 (4) | 0.100 (5) | 0.093 (4) | 0.002 (4) | −0.004 (4) | −0.006 (4) |
C35 | 0.080 (4) | 0.074 (5) | 0.130 (6) | −0.018 (3) | −0.020 (4) | −0.017 (4) |
Cd1—O2W | 2.250 (3) | C13—C14 | 1.396 (5) |
Cd1—O1 | 2.290 (3) | C13—C22 | 1.525 (5) |
Cd1—N2 | 2.353 (3) | C14—C20 | 1.433 (5) |
Cd1—N1 | 2.361 (3) | C14—H14A | 0.9623 |
Cd1—O1W | 2.385 (3) | C15—C16 | 1.385 (6) |
O1W—H1WA | 0.8623 | C15—C20 | 1.442 (5) |
O1W—H1WB | 0.8572 | C15—H15A | 0.9819 |
O2W—H2WA | 0.8675 | C16—C17 | 1.432 (6) |
O2W—H2WB | 0.8724 | C16—H16A | 0.9811 |
O1—C21 | 1.281 (5) | C17—C18 | 1.397 (6) |
O2—C21 | 1.294 (5) | C17—H17A | 0.9865 |
O3—C2 | 1.370 (4) | C18—C19 | 1.440 (5) |
O3—H3A | 0.8654 | C18—H18A | 0.9845 |
O4—C22 | 1.278 (5) | C19—C20 | 1.441 (5) |
O5—C22 | 1.286 (5) | C23—C24 | 1.393 (7) |
O6—C12 | 1.368 (4) | C23—H23A | 1.0014 |
O6—H6B | 0.8681 | C24—C25 | 1.390 (7) |
N1—C27 | 1.359 (5) | C24—H24A | 0.9894 |
N1—C23 | 1.365 (5) | C25—C26 | 1.397 (6) |
N2—C32 | 1.366 (5) | C25—H25A | 0.9813 |
N2—C28 | 1.370 (5) | C26—C27 | 1.413 (5) |
C1—C2 | 1.404 (5) | C26—H26A | 0.9946 |
C1—C9 | 1.437 (5) | C27—C28 | 1.513 (5) |
C1—C11 | 1.535 (5) | C28—C29 | 1.400 (5) |
C2—C3 | 1.466 (5) | C29—C30 | 1.399 (6) |
C3—C4 | 1.386 (5) | C29—H29A | 0.9869 |
C3—C21 | 1.509 (6) | C30—C31 | 1.393 (6) |
C4—C10 | 1.437 (5) | C30—H30A | 0.9833 |
C4—H4A | 0.9974 | C31—C32 | 1.394 (6) |
C5—C6 | 1.388 (6) | C31—H31A | 0.9831 |
C5—C10 | 1.439 (6) | C32—H32A | 0.9824 |
C5—H5A | 0.9977 | O7—C35 | 1.250 (7) |
C6—C7 | 1.435 (7) | N3—C35 | 1.345 (7) |
C6—H6A | 0.9804 | N3—C34 | 1.462 (6) |
C7—C8 | 1.374 (6) | N3—C33 | 1.473 (6) |
C7—H7A | 0.9744 | C33—H33A | 0.9612 |
C8—C9 | 1.442 (5) | C33—H33B | 0.9751 |
C8—H8A | 0.9985 | C33—H33C | 0.9645 |
C9—C10 | 1.439 (5) | C34—H34A | 0.9733 |
C11—C12 | 1.402 (5) | C34—H34B | 0.9652 |
C11—C19 | 1.452 (5) | C34—H34C | 0.9805 |
C12—C13 | 1.451 (5) | C35—H35A | 0.9976 |
O2W—Cd1—O1 | 134.74 (11) | C15—C16—C17 | 119.6 (4) |
O2W—Cd1—N2 | 102.48 (11) | C15—C16—H16A | 119.8 |
O1—Cd1—N2 | 99.38 (11) | C17—C16—H16A | 120.6 |
O2W—Cd1—N1 | 107.78 (11) | C18—C17—C16 | 120.7 (4) |
O1—Cd1—N1 | 116.62 (11) | C18—C17—H17A | 119.5 |
N2—Cd1—N1 | 71.57 (12) | C16—C17—H17A | 119.8 |
O2W—Cd1—O1W | 89.04 (11) | C17—C18—C19 | 121.0 (4) |
O1—Cd1—O1W | 82.13 (11) | C17—C18—H18A | 120.1 |
N2—Cd1—O1W | 161.24 (11) | C19—C18—H18A | 118.8 |
N1—Cd1—O1W | 90.93 (12) | C18—C19—C20 | 117.8 (4) |
Cd1—O1W—H1WA | 117.1 | C18—C19—C11 | 122.5 (4) |
Cd1—O1W—H1WB | 117.4 | C20—C19—C11 | 119.6 (4) |
H1WA—O1W—H1WB | 112.0 | C14—C20—C15 | 121.0 (4) |
Cd1—O2W—H2WA | 111.3 | C14—C20—C19 | 119.1 (4) |
Cd1—O2W—H2WB | 111.1 | C15—C20—C19 | 119.8 (4) |
H2WA—O2W—H2WB | 105.1 | O1—C21—O2 | 122.1 (4) |
C21—O1—Cd1 | 104.2 (3) | O1—C21—C3 | 119.2 (4) |
C2—O3—H3A | 119.6 | O2—C21—C3 | 118.7 (4) |
C12—O6—H6B | 120.1 | O4—C22—O5 | 124.1 (4) |
C27—N1—C23 | 119.7 (4) | O4—C22—C13 | 118.0 (4) |
C27—N1—Cd1 | 117.1 (3) | O5—C22—C13 | 117.9 (4) |
C23—N1—Cd1 | 123.1 (3) | N1—C23—C24 | 121.4 (4) |
C32—N2—C28 | 118.3 (3) | N1—C23—H23A | 119.5 |
C32—N2—Cd1 | 124.6 (3) | C24—C23—H23A | 119.1 |
C28—N2—Cd1 | 117.1 (3) | C25—C24—C23 | 119.6 (4) |
C2—C1—C9 | 119.4 (4) | C25—C24—H24A | 121.2 |
C2—C1—C11 | 120.5 (3) | C23—C24—H24A | 119.1 |
C9—C1—C11 | 120.1 (3) | C24—C25—C26 | 119.2 (4) |
O3—C2—C1 | 119.2 (4) | C24—C25—H25A | 120.1 |
O3—C2—C3 | 119.4 (4) | C26—C25—H25A | 120.7 |
C1—C2—C3 | 121.5 (4) | C25—C26—C27 | 119.3 (4) |
C4—C3—C2 | 117.6 (4) | C25—C26—H26A | 120.3 |
C4—C3—C21 | 120.9 (4) | C27—C26—H26A | 120.5 |
C2—C3—C21 | 121.5 (4) | N1—C27—C26 | 120.7 (4) |
C3—C4—C10 | 122.9 (4) | N1—C27—C28 | 117.3 (3) |
C3—C4—H4A | 118.5 | C26—C27—C28 | 122.0 (4) |
C10—C4—H4A | 118.6 | N2—C28—C29 | 121.3 (4) |
C6—C5—C10 | 121.0 (4) | N2—C28—C27 | 116.9 (3) |
C6—C5—H5A | 118.5 | C29—C28—C27 | 121.7 (4) |
C10—C5—H5A | 120.5 | C30—C29—C28 | 119.4 (4) |
C5—C6—C7 | 119.2 (4) | C30—C29—H29A | 120.3 |
C5—C6—H6A | 120.0 | C28—C29—H29A | 120.3 |
C7—C6—H6A | 120.8 | C31—C30—C29 | 119.7 (4) |
C8—C7—C6 | 121.0 (4) | C31—C30—H30A | 119.9 |
C8—C7—H7A | 120.4 | C29—C30—H30A | 120.4 |
C6—C7—H7A | 118.6 | C30—C31—C32 | 118.2 (4) |
C7—C8—C9 | 121.5 (4) | C30—C31—H31A | 121.4 |
C7—C8—H8A | 119.2 | C32—C31—H31A | 120.4 |
C9—C8—H8A | 119.3 | N2—C32—C31 | 123.1 (4) |
C1—C9—C10 | 120.1 (4) | N2—C32—H32A | 117.8 |
C1—C9—C8 | 122.3 (4) | C31—C32—H32A | 119.0 |
C10—C9—C8 | 117.6 (4) | C35—N3—C34 | 122.5 (5) |
C4—C10—C9 | 118.4 (4) | C35—N3—C33 | 120.7 (5) |
C4—C10—C5 | 122.0 (4) | C34—N3—C33 | 116.8 (5) |
C9—C10—C5 | 119.6 (4) | N3—C33—H33A | 110.4 |
C12—C11—C19 | 118.9 (3) | N3—C33—H33B | 110.4 |
C12—C11—C1 | 120.0 (3) | H33A—C33—H33B | 108.1 |
C19—C11—C1 | 121.1 (3) | N3—C33—H33C | 111.0 |
O6—C12—C11 | 118.6 (3) | H33A—C33—H33C | 109.0 |
O6—C12—C13 | 119.3 (3) | H33B—C33—H33C | 107.9 |
C11—C12—C13 | 122.1 (4) | N3—C34—H34A | 111.0 |
C14—C13—C12 | 118.2 (3) | N3—C34—H34B | 112.2 |
C14—C13—C22 | 120.7 (4) | H34A—C34—H34B | 107.9 |
C12—C13—C22 | 121.0 (4) | N3—C34—H34C | 111.3 |
C13—C14—C20 | 122.0 (4) | H34A—C34—H34C | 106.7 |
C13—C14—H14A | 119.1 | H34B—C34—H34C | 107.3 |
C20—C14—H14A | 118.9 | O7—C35—N3 | 126.2 (6) |
C16—C15—C20 | 120.9 (4) | O7—C35—H35A | 118.8 |
C16—C15—H15A | 120.4 | N3—C35—H35A | 115.1 |
C20—C15—H15A | 118.7 | ||
O2W—Cd1—O1—C21 | 37.9 (3) | C11—C12—C13—C22 | −179.0 (3) |
N2—Cd1—O1—C21 | −80.3 (3) | C12—C13—C14—C20 | −1.4 (6) |
N1—Cd1—O1—C21 | −154.3 (3) | C22—C13—C14—C20 | 179.8 (3) |
O1W—Cd1—O1—C21 | 118.6 (3) | C20—C15—C16—C17 | 0.2 (7) |
O2W—Cd1—N1—C27 | −96.3 (3) | C15—C16—C17—C18 | 0.0 (7) |
O1—Cd1—N1—C27 | 92.7 (3) | C16—C17—C18—C19 | 0.3 (7) |
N2—Cd1—N1—C27 | 1.3 (3) | C17—C18—C19—C20 | −0.9 (6) |
O1W—Cd1—N1—C27 | 174.4 (3) | C17—C18—C19—C11 | 178.7 (4) |
O2W—Cd1—N1—C23 | 80.5 (3) | C12—C11—C19—C18 | −179.6 (4) |
O1—Cd1—N1—C23 | −90.5 (3) | C1—C11—C19—C18 | −2.6 (6) |
N2—Cd1—N1—C23 | 178.1 (4) | C12—C11—C19—C20 | −0.1 (6) |
O1W—Cd1—N1—C23 | −8.8 (3) | C1—C11—C19—C20 | 176.9 (3) |
O2W—Cd1—N2—C32 | −75.3 (3) | C13—C14—C20—C15 | 179.3 (3) |
O1—Cd1—N2—C32 | 64.8 (3) | C13—C14—C20—C19 | −0.1 (6) |
N1—Cd1—N2—C32 | 179.9 (3) | C16—C15—C20—C14 | 179.9 (4) |
O1W—Cd1—N2—C32 | 157.9 (3) | C16—C15—C20—C19 | −0.7 (6) |
O2W—Cd1—N2—C28 | 104.5 (3) | C18—C19—C20—C14 | −179.5 (4) |
O1—Cd1—N2—C28 | −115.4 (3) | C11—C19—C20—C14 | 0.9 (6) |
N1—Cd1—N2—C28 | −0.3 (3) | C18—C19—C20—C15 | 1.1 (6) |
O1W—Cd1—N2—C28 | −22.2 (5) | C11—C19—C20—C15 | −178.5 (3) |
C9—C1—C2—O3 | 177.3 (3) | Cd1—O1—C21—O2 | 9.1 (5) |
C11—C1—C2—O3 | −4.6 (5) | Cd1—O1—C21—C3 | −169.8 (3) |
C9—C1—C2—C3 | −3.5 (5) | C4—C3—C21—O1 | −0.7 (6) |
C11—C1—C2—C3 | 174.6 (3) | C2—C3—C21—O1 | 176.2 (4) |
O3—C2—C3—C4 | −178.1 (4) | C4—C3—C21—O2 | −179.6 (4) |
C1—C2—C3—C4 | 2.6 (6) | C2—C3—C21—O2 | −2.8 (6) |
O3—C2—C3—C21 | 4.9 (6) | C14—C13—C22—O4 | −5.8 (6) |
C1—C2—C3—C21 | −174.3 (4) | C12—C13—C22—O4 | 175.4 (4) |
C2—C3—C4—C10 | 0.3 (6) | C14—C13—C22—O5 | 174.7 (4) |
C21—C3—C4—C10 | 177.3 (4) | C12—C13—C22—O5 | −4.1 (6) |
C10—C5—C6—C7 | −3.6 (7) | C27—N1—C23—C24 | −2.9 (7) |
C5—C6—C7—C8 | 1.8 (7) | Cd1—N1—C23—C24 | −179.6 (4) |
C6—C7—C8—C9 | −0.5 (7) | N1—C23—C24—C25 | 2.1 (8) |
C2—C1—C9—C10 | 1.4 (5) | C23—C24—C25—C26 | −1.3 (8) |
C11—C1—C9—C10 | −176.7 (3) | C24—C25—C26—C27 | 1.4 (7) |
C2—C1—C9—C8 | −176.5 (3) | C23—N1—C27—C26 | 2.9 (6) |
C11—C1—C9—C8 | 5.4 (6) | Cd1—N1—C27—C26 | 179.8 (3) |
C7—C8—C9—C1 | 178.8 (4) | C23—N1—C27—C28 | −179.0 (3) |
C7—C8—C9—C10 | 0.8 (6) | Cd1—N1—C27—C28 | −2.0 (4) |
C3—C4—C10—C9 | −2.3 (6) | C25—C26—C27—N1 | −2.2 (6) |
C3—C4—C10—C5 | 179.6 (4) | C25—C26—C27—C28 | 179.7 (4) |
C1—C9—C10—C4 | 1.4 (6) | C32—N2—C28—C29 | −0.6 (6) |
C8—C9—C10—C4 | 179.4 (4) | Cd1—N2—C28—C29 | 179.5 (3) |
C1—C9—C10—C5 | 179.5 (4) | C32—N2—C28—C27 | 179.2 (3) |
C8—C9—C10—C5 | −2.5 (6) | Cd1—N2—C28—C27 | −0.6 (4) |
C6—C5—C10—C4 | −178.0 (4) | N1—C27—C28—N2 | 1.8 (5) |
C6—C5—C10—C9 | 4.0 (7) | C26—C27—C28—N2 | 179.9 (3) |
C2—C1—C11—C12 | −106.7 (4) | N1—C27—C28—C29 | −178.3 (4) |
C9—C1—C11—C12 | 71.4 (5) | C26—C27—C28—C29 | −0.2 (6) |
C2—C1—C11—C19 | 76.3 (5) | N2—C28—C29—C30 | 0.0 (6) |
C9—C1—C11—C19 | −105.6 (4) | C27—C28—C29—C30 | −179.9 (4) |
C19—C11—C12—O6 | 179.9 (3) | C28—C29—C30—C31 | 0.6 (7) |
C1—C11—C12—O6 | 2.8 (5) | C29—C30—C31—C32 | −0.6 (7) |
C19—C11—C12—C13 | −1.5 (6) | C28—N2—C32—C31 | 0.6 (6) |
C1—C11—C12—C13 | −178.5 (3) | Cd1—N2—C32—C31 | −179.5 (3) |
O6—C12—C13—C14 | −179.1 (3) | C30—C31—C32—N2 | 0.0 (7) |
C11—C12—C13—C14 | 2.2 (6) | C34—N3—C35—O7 | 177.0 (6) |
O6—C12—C13—C22 | −0.3 (5) | C33—N3—C35—O7 | −1.4 (9) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2i | 0.86 | 2.37 | 3.225 (5) | 170 |
O1W—H1WB···O4ii | 0.86 | 2.00 | 2.792 (4) | 153 |
O2W—H2WB···O5ii | 0.87 | 2.37 | 3.052 (4) | 135 |
O2W—H2WB···O4ii | 0.87 | 2.56 | 3.372 (4) | 156 |
O3—H3A···O2 | 0.87 | 1.90 | 2.588 (4) | 135 |
O6—H6B···O5 | 0.87 | 1.86 | 2.553 (4) | 135 |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) −x+1, −y+2, −z. |