Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229618013967/sk3708sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229618013967/sk3708Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229618013967/sk3708sup3.pdf |
CCDC reference: 649523
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2008); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).
[Cd2(C14H14N2O6)2(H2O)4]·3H2O | F(000) = 972 |
Mr = 963.45 | Dx = 1.769 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.2072 (8) Å | Cell parameters from 8708 reflections |
b = 15.0256 (13) Å | θ = 2.7–27.4° |
c = 13.6139 (12) Å | µ = 1.26 mm−1 |
β = 106.177 (5)° | T = 298 K |
V = 1808.8 (3) Å3 | Sheet, colourless |
Z = 2 | 0.35 × 0.18 × 0.02 mm |
CCD area detector diffractometer | 6414 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.047 |
Bruker APEXII phi and ω scans | θmax = 27.5°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | h = −11→11 |
Tmin = 0.667, Tmax = 0.978 | k = −15→19 |
23758 measured reflections | l = −17→17 |
7584 independent reflections |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.033 | H-atom parameters constrained |
wR(F2) = 0.063 | w = 1/[σ2(Fo2) + (0.0238P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
7584 reflections | Δρmax = 0.39 e Å−3 |
482 parameters | Δρmin = −0.41 e Å−3 |
1 restraint | Absolute structure: Flack x determined using 2353 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.005 (16) |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Single-crystal X-ray diffraction measurements for the complex (I) was carried out on a Bruker APEXII CCD diffractometer with graphite monochromatized Mo Kα radiation (λ = 0.71073 Å) using both φ- and ω-scan modes at 298K. Data reduction was made with the SAINT package (Bruker, 2004). Absorption correction was performed using the SADABS program (Bruker, 2004). The structure was solved by direct method using SHELXS97 (Sheldrick, 2008) (and were refined on F2 by full-matrix least-squares using SHELXL2014/7 (Sheldrick, 2015) with anisotropic displacement parameters for all non-hydrogen atoms. |
x | y | z | Uiso*/Ueq | ||
C1 | 1.3890 (6) | 0.6046 (4) | 0.2117 (5) | 0.0261 (13) | |
C2 | 1.4564 (6) | 0.5330 (4) | 0.2909 (4) | 0.0265 (13) | |
H1 | 1.4558 | 0.5555 | 0.4363 | 0.032* | |
C3 | 1.6286 (6) | 0.5370 (4) | 0.3241 (5) | 0.0366 (15) | |
H3A | 1.6607 | 0.5933 | 0.3562 | 0.055* | |
H3B | 1.6660 | 0.5305 | 0.2653 | 0.055* | |
H3C | 1.6676 | 0.4898 | 0.3717 | 0.055* | |
H2 | 1.4270 | 0.4752 | 0.2585 | 0.044* | |
C4 | 1.2535 (6) | 0.5158 (4) | 0.3696 (5) | 0.0330 (14) | |
C5 | 0.9188 (6) | 0.3946 (4) | 0.8735 (5) | 0.0284 (14) | |
C6 | 1.0138 (5) | 0.4781 (4) | 0.8769 (4) | 0.0252 (11) | |
H6 | 0.9531 | 0.5298 | 0.8845 | 0.030* | |
C7 | 1.1518 (6) | 0.4713 (5) | 0.9711 (4) | 0.0353 (14) | |
H7A | 1.2114 | 0.4205 | 0.9642 | 0.053* | |
H7B | 1.1183 | 0.4648 | 1.0315 | 0.053* | |
H7C | 1.2118 | 0.5242 | 0.9765 | 0.053* | |
C8 | 0.9874 (6) | 0.5326 (4) | 0.7025 (5) | 0.0280 (13) | |
C9 | 1.0615 (6) | 0.5393 (4) | 0.6194 (5) | 0.0271 (13) | |
C10 | 1.2186 (6) | 0.5453 (4) | 0.6376 (5) | 0.0345 (15) | |
H10 | 1.2805 | 0.5528 | 0.7039 | 0.041* | |
C11 | 1.2803 (6) | 0.5407 (4) | 0.5572 (5) | 0.0357 (15) | |
H11 | 1.3847 | 0.5445 | 0.5697 | 0.043* | |
C12 | 1.1919 (6) | 0.5301 (4) | 0.4574 (5) | 0.0290 (13) | |
C13 | 1.0349 (7) | 0.5292 (5) | 0.4395 (5) | 0.0421 (17) | |
H13 | 0.9728 | 0.5257 | 0.3728 | 0.051* | |
C14 | 0.9725 (6) | 0.5344 (5) | 0.5192 (5) | 0.0379 (16) | |
H14 | 0.8678 | 0.5346 | 0.5058 | 0.046* | |
H16 | −0.6090 | 0.2931 | 0.1280 | 0.046* | |
C15 | −0.6171 (7) | 0.1575 (4) | 0.1357 (5) | 0.0283 (13) | |
C16 | −0.6231 (6) | 0.2510 (4) | 0.1792 (4) | 0.0311 (13) | |
C17 | −0.7734 (7) | 0.2727 (4) | 0.1994 (6) | 0.0487 (19) | |
H17A | −0.7941 | 0.2297 | 0.2460 | 0.073* | |
H17B | −0.8525 | 0.2709 | 0.1362 | 0.073* | |
H17C | −0.7687 | 0.3310 | 0.2288 | 0.073* | |
C18 | 0.4073 (6) | 0.3396 (4) | 0.8277 (4) | 0.0242 (12) | |
C19 | 0.3087 (5) | 0.2587 (4) | 0.7889 (4) | 0.0261 (13) | |
H19 | 0.3682 | 0.2165 | 0.7611 | 0.031* | |
C20 | 0.2706 (7) | 0.2144 (4) | 0.8778 (5) | 0.0419 (17) | |
H20A | 0.2083 | 0.2533 | 0.9045 | 0.063* | |
H20B | 0.3622 | 0.2016 | 0.9302 | 0.063* | |
H20C | 0.2172 | 0.1599 | 0.8552 | 0.063* | |
C21 | 0.1702 (6) | 0.2773 (4) | 0.6099 (5) | 0.0301 (14) | |
C22 | 0.0245 (6) | 0.2885 (4) | 0.5272 (5) | 0.0283 (13) | |
C23 | 0.0360 (7) | 0.3028 (5) | 0.4298 (5) | 0.0400 (16) | |
H23 | 0.1308 | 0.3094 | 0.4191 | 0.048* | |
C24 | −0.0923 (7) | 0.3074 (5) | 0.3474 (5) | 0.0383 (16) | |
H24 | −0.0831 | 0.3167 | 0.2819 | 0.046* | |
C25 | −0.2346 (6) | 0.2983 (4) | 0.3615 (5) | 0.0288 (13) | |
C26 | −0.2464 (6) | 0.2852 (4) | 0.4596 (5) | 0.0370 (15) | |
H26 | −0.3413 | 0.2795 | 0.4706 | 0.044* | |
C27 | −0.1170 (6) | 0.2805 (5) | 0.5424 (5) | 0.0394 (16) | |
H27 | −0.1263 | 0.2719 | 0.6080 | 0.047* | |
C28 | −0.3671 (6) | 0.3012 (4) | 0.2682 (5) | 0.0285 (13) | |
Cd1 | 0.76277 (4) | 0.24331 (3) | 0.90938 (3) | 0.02744 (11) | |
Cd2 | 0.60257 (4) | 0.47990 (2) | 0.89586 (3) | 0.02782 (11) | |
N1 | 1.3982 (5) | 0.5383 (3) | 0.3784 (4) | 0.0309 (12) | |
N2 | 1.0652 (5) | 0.4901 (3) | 0.7865 (3) | 0.0282 (11) | |
H2A | 1.1520 | 0.4684 | 0.7871 | 0.034* | |
N3 | 0.1709 (5) | 0.2796 (3) | 0.7071 (4) | 0.0292 (11) | |
H3D | 0.0896 | 0.2937 | 0.7228 | 0.035* | |
N4 | −0.4960 (5) | 0.2630 (3) | 0.2707 (4) | 0.0316 (13) | |
H4 | −0.5056 | 0.2449 | 0.3284 | 0.038* | |
O1 | 1.3177 (5) | 0.6683 (3) | 0.2377 (4) | 0.0372 (11) | |
O2 | 1.4095 (5) | 0.5994 (3) | 0.1252 (3) | 0.0364 (11) | |
O3 | 0.9219 (4) | 0.3315 (3) | 0.8160 (4) | 0.0399 (11) | |
O4 | 0.8414 (5) | 0.3919 (3) | 0.9386 (4) | 0.0383 (11) | |
O5 | 0.5416 (4) | 0.3262 (3) | 0.8796 (3) | 0.0359 (11) | |
O6 | 0.3558 (4) | 0.4169 (3) | 0.8126 (3) | 0.0336 (10) | |
O7 | −0.4904 (5) | 0.1242 (3) | 0.1396 (4) | 0.0378 (12) | |
O8 | −0.7386 (5) | 0.1166 (3) | 0.0978 (3) | 0.0334 (11) | |
O9 | 0.5739 (6) | 0.4792 (4) | 1.0541 (3) | 0.0564 (13) | |
H9A | 0.5676 | 0.4258 | 1.0730 | 0.085* | |
H9B | 0.6499 | 0.5042 | 1.0948 | 0.085* | |
O10 | 0.6232 (4) | 0.4802 (3) | 0.7334 (3) | 0.0392 (10) | |
H10A | 0.6227 | 0.4268 | 0.7127 | 0.059* | |
H10B | 0.7058 | 0.5051 | 0.7326 | 0.059* | |
O11 | 0.7439 (5) | 0.2162 (3) | 1.0698 (3) | 0.0436 (14) | |
H11A | 0.7936 | 0.2556 | 1.1103 | 0.065* | |
H11B | 0.6516 | 0.2182 | 1.0696 | 0.065* | |
O12 | 0.9751 (5) | 0.1574 (3) | 0.9594 (4) | 0.0446 (12) | |
H12A | 1.0524 | 0.1910 | 0.9759 | 0.067* | |
H12B | 0.9803 | 0.1238 | 0.9103 | 0.067* | |
O13 | 1.1767 (5) | 0.4815 (4) | 0.2894 (3) | 0.0514 (12) | |
O14 | 0.2887 (4) | 0.2626 (3) | 0.5849 (3) | 0.0420 (12) | |
O15 | −0.3518 (5) | 0.3372 (3) | 0.1891 (3) | 0.0369 (10) | |
O16 | 0.8588 (4) | 0.5628 (3) | 0.6929 (4) | 0.0402 (11) | |
O17 | 0.5818 (5) | 0.3219 (3) | 0.6348 (4) | 0.0530 (13) | |
H17D | 0.6471 | 0.2850 | 0.6680 | 0.079* | |
H17E | 0.4936 | 0.3027 | 0.6309 | 0.079* | |
O18 | 0.3934 (5) | 0.1585 (3) | 0.4420 (4) | 0.0499 (13) | |
H18A | 0.3224 | 0.1282 | 0.4032 | 0.060* | |
H18B | 0.3592 | 0.2011 | 0.4702 | 0.060* | |
O19 | 0.0696 (6) | 0.0226 (5) | 0.8597 (5) | 0.087 (2) | |
H19A | 0.0496 | 0.0053 | 0.7979 | 0.105* | |
H19B | 0.1072 | −0.0214 | 0.8975 | 0.105* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.023 (3) | 0.030 (3) | 0.024 (3) | −0.007 (2) | 0.004 (2) | −0.001 (3) |
C2 | 0.031 (3) | 0.024 (3) | 0.027 (3) | −0.003 (2) | 0.011 (2) | 0.003 (3) |
C3 | 0.032 (3) | 0.038 (4) | 0.037 (4) | 0.004 (3) | 0.007 (3) | 0.000 (3) |
C4 | 0.035 (3) | 0.030 (3) | 0.034 (4) | 0.000 (3) | 0.011 (3) | 0.000 (3) |
C5 | 0.015 (3) | 0.036 (4) | 0.032 (4) | 0.002 (2) | 0.004 (2) | 0.009 (3) |
C6 | 0.024 (3) | 0.025 (3) | 0.029 (3) | −0.001 (3) | 0.010 (2) | −0.003 (3) |
C7 | 0.030 (3) | 0.045 (4) | 0.029 (3) | −0.006 (3) | 0.004 (2) | −0.002 (3) |
C8 | 0.025 (3) | 0.027 (3) | 0.031 (4) | −0.003 (2) | 0.006 (2) | 0.003 (3) |
C9 | 0.026 (3) | 0.027 (3) | 0.030 (3) | 0.002 (2) | 0.012 (2) | 0.004 (3) |
C10 | 0.029 (3) | 0.046 (4) | 0.028 (4) | −0.006 (3) | 0.008 (3) | 0.007 (3) |
C11 | 0.021 (3) | 0.051 (4) | 0.035 (4) | −0.009 (3) | 0.008 (3) | 0.006 (3) |
C12 | 0.033 (3) | 0.023 (3) | 0.034 (4) | −0.001 (2) | 0.012 (3) | 0.003 (3) |
C13 | 0.035 (3) | 0.058 (5) | 0.031 (4) | −0.001 (3) | 0.005 (3) | 0.001 (3) |
C14 | 0.022 (3) | 0.057 (4) | 0.035 (4) | 0.005 (3) | 0.007 (3) | 0.000 (3) |
C15 | 0.038 (3) | 0.024 (3) | 0.021 (3) | −0.003 (2) | 0.005 (3) | 0.001 (2) |
C16 | 0.034 (3) | 0.026 (3) | 0.027 (3) | 0.002 (3) | −0.001 (2) | 0.001 (3) |
C17 | 0.036 (3) | 0.041 (4) | 0.065 (5) | 0.008 (3) | 0.007 (3) | −0.013 (4) |
C18 | 0.019 (3) | 0.029 (3) | 0.027 (3) | 0.003 (2) | 0.011 (2) | −0.002 (3) |
C19 | 0.019 (2) | 0.030 (3) | 0.028 (3) | 0.002 (2) | 0.003 (2) | −0.002 (3) |
C20 | 0.040 (4) | 0.043 (4) | 0.041 (4) | −0.002 (3) | 0.008 (3) | 0.013 (3) |
C21 | 0.025 (3) | 0.030 (3) | 0.035 (4) | 0.001 (2) | 0.008 (3) | −0.001 (3) |
C22 | 0.025 (3) | 0.031 (3) | 0.027 (3) | 0.000 (2) | 0.005 (2) | −0.003 (3) |
C23 | 0.027 (3) | 0.056 (4) | 0.038 (4) | 0.000 (3) | 0.011 (3) | 0.004 (3) |
C24 | 0.038 (3) | 0.053 (4) | 0.025 (4) | −0.004 (3) | 0.012 (3) | 0.007 (3) |
C25 | 0.028 (3) | 0.028 (3) | 0.028 (3) | −0.001 (2) | 0.005 (2) | −0.002 (3) |
C26 | 0.025 (3) | 0.059 (4) | 0.029 (4) | −0.002 (3) | 0.010 (3) | 0.001 (3) |
C27 | 0.028 (3) | 0.068 (5) | 0.022 (3) | −0.004 (3) | 0.007 (2) | −0.004 (3) |
C28 | 0.035 (3) | 0.024 (3) | 0.026 (3) | 0.004 (2) | 0.007 (3) | 0.000 (3) |
Cd1 | 0.02478 (19) | 0.0263 (2) | 0.0301 (2) | 0.00085 (18) | 0.00565 (16) | −0.0015 (2) |
Cd2 | 0.0275 (2) | 0.0265 (2) | 0.0304 (2) | −0.00243 (18) | 0.00971 (17) | 0.0005 (2) |
N1 | 0.029 (3) | 0.038 (3) | 0.026 (3) | −0.002 (2) | 0.008 (2) | 0.003 (2) |
N2 | 0.025 (2) | 0.032 (3) | 0.032 (3) | 0.003 (2) | 0.0145 (19) | 0.004 (3) |
N3 | 0.021 (2) | 0.036 (3) | 0.030 (3) | 0.0000 (19) | 0.006 (2) | −0.006 (2) |
N4 | 0.034 (3) | 0.036 (3) | 0.022 (3) | −0.006 (2) | 0.004 (2) | 0.001 (2) |
O1 | 0.041 (2) | 0.030 (3) | 0.043 (3) | 0.0112 (19) | 0.016 (2) | 0.008 (2) |
O2 | 0.039 (3) | 0.043 (3) | 0.025 (3) | −0.001 (2) | 0.007 (2) | 0.006 (2) |
O3 | 0.035 (2) | 0.033 (3) | 0.052 (3) | −0.0039 (18) | 0.012 (2) | −0.007 (2) |
O4 | 0.029 (2) | 0.043 (3) | 0.046 (3) | −0.0003 (19) | 0.014 (2) | 0.011 (2) |
O5 | 0.019 (2) | 0.031 (3) | 0.050 (3) | 0.0013 (17) | −0.0029 (19) | −0.005 (2) |
O6 | 0.023 (2) | 0.031 (2) | 0.047 (3) | 0.0025 (17) | 0.0087 (18) | 0.004 (2) |
O7 | 0.027 (2) | 0.035 (3) | 0.051 (3) | 0.0040 (19) | 0.010 (2) | −0.002 (2) |
O8 | 0.030 (2) | 0.031 (3) | 0.038 (3) | −0.0029 (18) | 0.008 (2) | −0.001 (2) |
O9 | 0.095 (4) | 0.043 (3) | 0.038 (3) | 0.015 (3) | 0.031 (3) | 0.009 (3) |
O10 | 0.038 (2) | 0.044 (3) | 0.040 (3) | −0.009 (2) | 0.0167 (19) | 0.001 (3) |
O11 | 0.043 (3) | 0.052 (4) | 0.037 (3) | 0.001 (2) | 0.012 (2) | −0.002 (2) |
O12 | 0.032 (2) | 0.049 (3) | 0.053 (3) | 0.007 (2) | 0.011 (2) | 0.005 (2) |
O13 | 0.041 (2) | 0.069 (3) | 0.045 (3) | −0.013 (3) | 0.013 (2) | −0.020 (3) |
O14 | 0.0234 (19) | 0.068 (4) | 0.036 (3) | 0.003 (2) | 0.0106 (18) | −0.005 (2) |
O15 | 0.042 (2) | 0.041 (3) | 0.028 (2) | 0.0016 (19) | 0.010 (2) | 0.004 (2) |
O16 | 0.024 (2) | 0.052 (3) | 0.047 (3) | 0.0112 (19) | 0.013 (2) | 0.014 (2) |
O17 | 0.039 (3) | 0.075 (4) | 0.047 (3) | −0.009 (2) | 0.016 (2) | −0.007 (3) |
O18 | 0.042 (3) | 0.056 (3) | 0.051 (3) | −0.003 (2) | 0.012 (2) | −0.017 (3) |
O19 | 0.067 (4) | 0.104 (6) | 0.081 (5) | −0.006 (4) | 0.006 (3) | −0.022 (4) |
C1—O2 | 1.246 (7) | C21—O14 | 1.249 (6) |
C1—O1 | 1.265 (7) | C21—N3 | 1.322 (7) |
C1—C2 | 1.527 (8) | C21—C22 | 1.502 (8) |
C2—N1 | 1.440 (7) | C22—C23 | 1.375 (9) |
C2—C3 | 1.524 (8) | C22—C27 | 1.380 (8) |
C2—H2 | 0.9774 | C23—C24 | 1.386 (8) |
C3—H3A | 0.9600 | C23—H23 | 0.9300 |
C3—H3B | 0.9600 | C24—C25 | 1.383 (8) |
C3—H3C | 0.9600 | C24—H24 | 0.9300 |
C4—O13 | 1.236 (7) | C25—C26 | 1.384 (8) |
C4—N1 | 1.346 (7) | C25—C28 | 1.497 (7) |
C4—C12 | 1.475 (8) | C26—C27 | 1.395 (8) |
C5—O3 | 1.235 (7) | C26—H26 | 0.9299 |
C5—O4 | 1.283 (7) | C27—H27 | 0.9301 |
C5—C6 | 1.523 (8) | C28—O15 | 1.248 (7) |
C6—N2 | 1.447 (7) | C28—N4 | 1.327 (7) |
C6—C7 | 1.537 (7) | Cd1—O1ii | 2.237 (4) |
C6—H6 | 0.9801 | Cd1—O11 | 2.276 (4) |
C7—H7A | 0.9600 | Cd1—O12 | 2.282 (4) |
C7—H7B | 0.9600 | Cd1—O5 | 2.324 (4) |
C7—H7C | 0.9600 | Cd1—O4 | 2.347 (4) |
C8—O16 | 1.240 (6) | Cd1—O3 | 2.561 (4) |
C8—N2 | 1.331 (7) | Cd1—O2ii | 2.645 (5) |
C8—C9 | 1.479 (8) | Cd2—O9 | 2.242 (4) |
C9—C14 | 1.383 (8) | Cd2—O10 | 2.271 (4) |
C9—C10 | 1.401 (7) | Cd2—O5 | 2.372 (4) |
C10—C11 | 1.369 (8) | Cd2—O7iii | 2.393 (4) |
C10—H10 | 0.9300 | Cd2—O8iii | 2.396 (4) |
C11—C12 | 1.384 (8) | Cd2—O6 | 2.431 (4) |
C11—H11 | 0.9300 | Cd2—O4 | 2.492 (4) |
C12—C13 | 1.397 (8) | Cd2—C15iii | 2.712 (6) |
C13—C14 | 1.365 (8) | N1—H1 | 0.8583 |
C13—H13 | 0.9300 | N2—H2A | 0.8601 |
C14—H14 | 0.9300 | N3—H3D | 0.8600 |
C15—O8 | 1.254 (7) | N4—H4 | 0.8600 |
C15—O7 | 1.257 (7) | O1—Cd1iv | 2.237 (4) |
C15—C16 | 1.532 (8) | O2—Cd1iv | 2.645 (5) |
C15—Cd2i | 2.712 (6) | O7—Cd2i | 2.393 (4) |
C16—N4 | 1.463 (6) | O8—Cd2i | 2.396 (4) |
C16—C17 | 1.520 (8) | O9—H9A | 0.8501 |
C16—H16 | 0.9775 | O9—H9B | 0.8500 |
C17—H17A | 0.9600 | O10—H10A | 0.8499 |
C17—H17B | 0.9600 | O10—H10B | 0.8500 |
C17—H17C | 0.9600 | O11—H11A | 0.8500 |
C18—O6 | 1.250 (6) | O11—H11B | 0.8499 |
C18—O5 | 1.258 (6) | O12—H12A | 0.8500 |
C18—C19 | 1.521 (7) | O12—H12B | 0.8500 |
C18—Cd2 | 2.759 (5) | O17—H17D | 0.8501 |
C19—N3 | 1.470 (6) | O17—H17E | 0.8499 |
C19—C20 | 1.505 (8) | O18—H18A | 0.8500 |
C19—H19 | 0.9799 | O18—H18B | 0.8499 |
C20—H20A | 0.9600 | O19—H19A | 0.8500 |
C20—H20B | 0.9600 | O19—H19B | 0.8500 |
C20—H20C | 0.9600 | ||
O2—C1—O1 | 122.6 (6) | C25—C26—C27 | 120.5 (5) |
O2—C1—C2 | 118.9 (5) | C25—C26—H26 | 119.8 |
O1—C1—C2 | 118.4 (5) | C27—C26—H26 | 119.7 |
N1—C2—C3 | 110.4 (5) | C22—C27—C26 | 120.3 (6) |
N1—C2—C1 | 111.9 (5) | C22—C27—H27 | 120.0 |
C3—C2—C1 | 111.5 (5) | C26—C27—H27 | 119.7 |
N1—C2—H2 | 107.6 | O15—C28—N4 | 121.7 (5) |
C3—C2—H2 | 107.7 | O15—C28—C25 | 118.9 (5) |
C1—C2—H2 | 107.5 | N4—C28—C25 | 119.3 (5) |
C2—C3—H3A | 109.5 | O1ii—Cd1—O11 | 132.41 (16) |
C2—C3—H3B | 109.5 | O1ii—Cd1—O12 | 91.42 (17) |
H3A—C3—H3B | 109.5 | O11—Cd1—O12 | 84.26 (16) |
C2—C3—H3C | 109.5 | O1ii—Cd1—O5 | 93.34 (15) |
H3A—C3—H3C | 109.5 | O11—Cd1—O5 | 88.07 (16) |
H3B—C3—H3C | 109.5 | O12—Cd1—O5 | 172.31 (17) |
O13—C4—N1 | 119.5 (6) | O1ii—Cd1—O4 | 129.84 (16) |
O13—C4—C12 | 121.4 (5) | O11—Cd1—O4 | 96.33 (17) |
N1—C4—C12 | 119.1 (5) | O12—Cd1—O4 | 106.83 (16) |
O3—C5—O4 | 122.0 (6) | O5—Cd1—O4 | 74.54 (14) |
O3—C5—C6 | 122.5 (5) | O1ii—Cd1—O3 | 84.76 (15) |
O4—C5—C6 | 115.4 (5) | O11—Cd1—O3 | 140.94 (16) |
N2—C6—C5 | 113.5 (5) | O12—Cd1—O3 | 83.11 (15) |
N2—C6—C7 | 109.1 (4) | O5—Cd1—O3 | 103.33 (15) |
C5—C6—C7 | 107.7 (5) | O4—Cd1—O3 | 53.10 (15) |
N2—C6—H6 | 108.8 | O1ii—Cd1—O2ii | 52.86 (15) |
C5—C6—H6 | 108.5 | O11—Cd1—O2ii | 79.75 (16) |
C7—C6—H6 | 109.1 | O12—Cd1—O2ii | 90.69 (15) |
C6—C7—H7A | 109.5 | O5—Cd1—O2ii | 87.38 (14) |
C6—C7—H7B | 109.5 | O4—Cd1—O2ii | 161.67 (14) |
H7A—C7—H7B | 109.5 | O3—Cd1—O2ii | 137.08 (14) |
C6—C7—H7C | 109.5 | O9—Cd2—O10 | 178.12 (16) |
H7A—C7—H7C | 109.5 | O9—Cd2—O5 | 89.84 (18) |
H7B—C7—H7C | 109.5 | O10—Cd2—O5 | 89.58 (17) |
O16—C8—N2 | 122.4 (6) | O9—Cd2—O7iii | 92.20 (18) |
O16—C8—C9 | 121.6 (5) | O10—Cd2—O7iii | 87.15 (17) |
N2—C8—C9 | 115.9 (5) | O5—Cd2—O7iii | 141.80 (14) |
C14—C9—C10 | 118.5 (6) | O9—Cd2—O8iii | 99.79 (18) |
C14—C9—C8 | 118.5 (5) | O10—Cd2—O8iii | 81.28 (16) |
C10—C9—C8 | 122.9 (5) | O5—Cd2—O8iii | 161.09 (14) |
C11—C10—C9 | 119.5 (6) | O7iii—Cd2—O8iii | 54.68 (14) |
C11—C10—H10 | 120.3 | O9—Cd2—O6 | 95.81 (17) |
C9—C10—H10 | 120.2 | O10—Cd2—O6 | 82.41 (14) |
C10—C11—C12 | 122.0 (5) | O5—Cd2—O6 | 53.92 (13) |
C10—C11—H11 | 119.2 | O7iii—Cd2—O6 | 87.94 (14) |
C12—C11—H11 | 118.9 | O8iii—Cd2—O6 | 139.68 (14) |
C11—C12—C13 | 118.0 (6) | O9—Cd2—O4 | 96.07 (16) |
C11—C12—C4 | 123.9 (5) | O10—Cd2—O4 | 85.43 (15) |
C13—C12—C4 | 118.1 (5) | O5—Cd2—O4 | 71.08 (14) |
C14—C13—C12 | 120.3 (6) | O7iii—Cd2—O4 | 146.22 (14) |
C14—C13—H13 | 120.0 | O8iii—Cd2—O4 | 91.60 (14) |
C12—C13—H13 | 119.7 | O6—Cd2—O4 | 123.48 (14) |
C13—C14—C9 | 121.5 (5) | O9—Cd2—C15iii | 100.44 (19) |
C13—C14—H14 | 119.1 | O10—Cd2—C15iii | 79.77 (18) |
C9—C14—H14 | 119.4 | O5—Cd2—C15iii | 164.54 (16) |
O8—C15—O7 | 122.3 (6) | O7iii—Cd2—C15iii | 27.61 (15) |
O8—C15—C16 | 118.9 (5) | O8iii—Cd2—C15iii | 27.54 (15) |
O7—C15—C16 | 118.8 (5) | O6—Cd2—C15iii | 112.98 (16) |
O8—C15—Cd2i | 62.1 (3) | O4—Cd2—C15iii | 118.65 (16) |
O7—C15—Cd2i | 61.9 (3) | O9—Cd2—C18 | 94.56 (19) |
C16—C15—Cd2i | 166.6 (4) | O10—Cd2—C18 | 84.12 (17) |
N4—C16—C17 | 111.9 (5) | O5—Cd2—C18 | 27.07 (14) |
N4—C16—C15 | 109.7 (5) | O7iii—Cd2—C18 | 114.87 (16) |
C17—C16—C15 | 113.5 (5) | O8iii—Cd2—C18 | 162.35 (15) |
N4—C16—H16 | 107.1 | O6—Cd2—C18 | 26.92 (14) |
C17—C16—H16 | 107.4 | O4—Cd2—C18 | 97.08 (15) |
C15—C16—H16 | 107.0 | C15iii—Cd2—C18 | 139.03 (17) |
C16—C17—H17A | 109.5 | C4—N1—C2 | 120.0 (5) |
C16—C17—H17B | 109.5 | C4—N1—H1 | 120.0 |
H17A—C17—H17B | 109.5 | C2—N1—H1 | 120.0 |
C16—C17—H17C | 109.5 | C8—N2—C6 | 124.4 (5) |
H17A—C17—H17C | 109.5 | C8—N2—H2A | 117.8 |
H17B—C17—H17C | 109.5 | C6—N2—H2A | 117.9 |
O6—C18—O5 | 120.6 (5) | C21—N3—C19 | 121.0 (5) |
O6—C18—C19 | 121.6 (5) | C21—N3—H3D | 119.6 |
O5—C18—C19 | 117.8 (5) | C19—N3—H3D | 119.5 |
O6—C18—Cd2 | 61.8 (3) | C28—N4—C16 | 122.8 (5) |
O5—C18—Cd2 | 59.1 (3) | C28—N4—H4 | 118.7 |
C19—C18—Cd2 | 176.1 (4) | C16—N4—H4 | 118.5 |
N3—C19—C20 | 111.0 (4) | C1—O1—Cd1iv | 101.4 (4) |
N3—C19—C18 | 113.4 (5) | C1—O2—Cd1iv | 82.9 (4) |
C20—C19—C18 | 108.9 (5) | C5—O3—Cd1 | 88.0 (4) |
N3—C19—H19 | 107.7 | C5—O4—Cd1 | 96.7 (4) |
C20—C19—H19 | 107.7 | C5—O4—Cd2 | 116.5 (3) |
C18—C19—H19 | 107.9 | Cd1—O4—Cd2 | 104.75 (15) |
C19—C20—H20A | 109.5 | C18—O5—Cd1 | 149.3 (4) |
C19—C20—H20B | 109.5 | C18—O5—Cd2 | 93.9 (3) |
H20A—C20—H20B | 109.5 | Cd1—O5—Cd2 | 109.42 (16) |
C19—C20—H20C | 109.5 | C18—O6—Cd2 | 91.3 (3) |
H20A—C20—H20C | 109.5 | C15—O7—Cd2i | 90.5 (3) |
H20B—C20—H20C | 109.5 | C15—O8—Cd2i | 90.4 (4) |
O14—C21—N3 | 121.1 (5) | Cd2—O9—H9A | 109.4 |
O14—C21—C22 | 118.7 (6) | Cd2—O9—H9B | 109.2 |
N3—C21—C22 | 120.1 (5) | H9A—O9—H9B | 109.5 |
C23—C22—C27 | 119.2 (5) | Cd2—O10—H10A | 109.1 |
C23—C22—C21 | 116.6 (5) | Cd2—O10—H10B | 109.4 |
C27—C22—C21 | 124.1 (6) | H10A—O10—H10B | 109.5 |
C22—C23—C24 | 120.7 (6) | Cd1—O11—H11A | 109.1 |
C22—C23—H23 | 119.7 | Cd1—O11—H11B | 109.5 |
C24—C23—H23 | 119.6 | H11A—O11—H11B | 109.5 |
C25—C24—C23 | 120.6 (6) | Cd1—O12—H12A | 109.1 |
C25—C24—H24 | 119.5 | Cd1—O12—H12B | 109.4 |
C23—C24—H24 | 119.9 | H12A—O12—H12B | 109.5 |
C24—C25—C26 | 118.7 (5) | H17D—O17—H17E | 109.5 |
C24—C25—C28 | 117.3 (6) | H18A—O18—H18B | 111.6 |
C26—C25—C28 | 124.0 (5) | H19A—O19—H19B | 107.5 |
O2—C1—C2—N1 | −168.4 (5) | C28—C25—C26—C27 | 177.9 (6) |
O1—C1—C2—N1 | 13.4 (7) | C23—C22—C27—C26 | 1.2 (10) |
O2—C1—C2—C3 | 67.4 (6) | C21—C22—C27—C26 | −175.1 (6) |
O1—C1—C2—C3 | −110.8 (6) | C25—C26—C27—C22 | −0.3 (10) |
O3—C5—C6—N2 | 19.8 (7) | C24—C25—C28—O15 | −21.4 (8) |
O4—C5—C6—N2 | −163.9 (5) | C26—C25—C28—O15 | 160.0 (6) |
O3—C5—C6—C7 | −101.1 (6) | C24—C25—C28—N4 | 156.5 (6) |
O4—C5—C6—C7 | 75.2 (6) | C26—C25—C28—N4 | −22.1 (9) |
O16—C8—C9—C14 | −33.8 (9) | O13—C4—N1—C2 | 8.0 (9) |
N2—C8—C9—C14 | 144.3 (6) | C12—C4—N1—C2 | −174.0 (5) |
O16—C8—C9—C10 | 149.8 (6) | C3—C2—N1—C4 | −164.9 (5) |
N2—C8—C9—C10 | −32.0 (8) | C1—C2—N1—C4 | 70.3 (7) |
C14—C9—C10—C11 | −4.1 (9) | O16—C8—N2—C6 | −3.2 (9) |
C8—C9—C10—C11 | 172.2 (6) | C9—C8—N2—C6 | 178.7 (5) |
C9—C10—C11—C12 | 0.1 (10) | C5—C6—N2—C8 | 88.3 (7) |
C10—C11—C12—C13 | 3.4 (9) | C7—C6—N2—C8 | −151.6 (5) |
C10—C11—C12—C4 | −173.7 (6) | O14—C21—N3—C19 | −4.4 (8) |
O13—C4—C12—C11 | 158.4 (7) | C22—C21—N3—C19 | 173.0 (5) |
N1—C4—C12—C11 | −19.5 (9) | C20—C19—N3—C21 | −147.0 (5) |
O13—C4—C12—C13 | −18.7 (9) | C18—C19—N3—C21 | 89.9 (6) |
N1—C4—C12—C13 | 163.3 (6) | O15—C28—N4—C16 | 7.3 (9) |
C11—C12—C13—C14 | −3.0 (10) | C25—C28—N4—C16 | −170.5 (5) |
C4—C12—C13—C14 | 174.3 (6) | C17—C16—N4—C28 | −137.6 (6) |
C12—C13—C14—C9 | −1.1 (10) | C15—C16—N4—C28 | 95.5 (6) |
C10—C9—C14—C13 | 4.6 (10) | O2—C1—O1—Cd1iv | 5.3 (6) |
C8—C9—C14—C13 | −171.9 (6) | C2—C1—O1—Cd1iv | −176.7 (4) |
O8—C15—C16—N4 | 143.0 (5) | O1—C1—O2—Cd1iv | −4.4 (5) |
O7—C15—C16—N4 | −36.8 (7) | C2—C1—O2—Cd1iv | 177.5 (4) |
Cd2i—C15—C16—N4 | 52.5 (19) | O4—C5—O3—Cd1 | −4.7 (5) |
O8—C15—C16—C17 | 17.1 (8) | C6—C5—O3—Cd1 | 171.4 (5) |
O7—C15—C16—C17 | −162.7 (6) | O3—C5—O4—Cd1 | 5.1 (6) |
Cd2i—C15—C16—C17 | −73.4 (18) | C6—C5—O4—Cd1 | −171.2 (4) |
O6—C18—C19—N3 | 19.0 (8) | O3—C5—O4—Cd2 | −105.1 (5) |
O5—C18—C19—N3 | −164.0 (5) | C6—C5—O4—Cd2 | 78.6 (5) |
O6—C18—C19—C20 | −105.1 (6) | O6—C18—O5—Cd1 | −145.7 (6) |
O5—C18—C19—C20 | 71.9 (7) | C19—C18—O5—Cd1 | 37.2 (11) |
O14—C21—C22—C23 | −14.9 (8) | Cd2—C18—O5—Cd1 | −140.1 (8) |
N3—C21—C22—C23 | 167.7 (6) | O6—C18—O5—Cd2 | −5.6 (6) |
O14—C21—C22—C27 | 161.5 (6) | C19—C18—O5—Cd2 | 177.3 (4) |
N3—C21—C22—C27 | −16.0 (9) | O5—C18—O6—Cd2 | 5.5 (6) |
C27—C22—C23—C24 | −1.3 (10) | C19—C18—O6—Cd2 | −177.6 (5) |
C21—C22—C23—C24 | 175.3 (6) | O8—C15—O7—Cd2i | −15.1 (6) |
C22—C23—C24—C25 | 0.4 (10) | C16—C15—O7—Cd2i | 164.7 (5) |
C23—C24—C25—C26 | 0.6 (10) | O7—C15—O8—Cd2i | 15.0 (6) |
C23—C24—C25—C28 | −178.1 (6) | C16—C15—O8—Cd2i | −164.7 (5) |
C24—C25—C26—C27 | −0.6 (10) |
Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x+2, y−1/2, −z+1; (iii) −x, y+1/2, −z+1; (iv) −x+2, y+1/2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O18iv | 0.86 | 2.40 | 3.210 (7) | 156 |
N2—H2A···O6v | 0.86 | 1.97 | 2.822 (6) | 171 |
N3—H3D···O3vi | 0.86 | 2.33 | 3.155 (6) | 162 |
N4—H4···O18vi | 0.86 | 2.40 | 3.205 (7) | 157 |
O9—H9A···O15vii | 0.85 | 2.04 | 2.775 (6) | 144 |
O9—H9B···O19viii | 0.85 | 2.50 | 3.229 (8) | 145 |
O10—H10A···O17 | 0.85 | 1.88 | 2.706 (7) | 164 |
O10—H10B···O16 | 0.85 | 1.86 | 2.687 (6) | 164 |
O11—H11A···O15vii | 0.85 | 2.29 | 2.742 (6) | 113 |
O11—H11B···O7vii | 0.85 | 2.30 | 2.934 (6) | 131 |
O11—H11A···O15vii | 0.85 | 2.29 | 2.742 (6) | 113 |
O12—H12A···O8ix | 0.85 | 2.43 | 2.847 (6) | 111 |
O12—H12B···O19v | 0.85 | 1.94 | 2.713 (8) | 150 |
O17—H17D···O1ii | 0.85 | 2.14 | 2.881 (7) | 145 |
O17—H17E···O14 | 0.85 | 1.91 | 2.742 (6) | 165 |
O18—H18A···O16x | 0.85 | 2.06 | 2.908 (6) | 176 |
O18—H18B···O14 | 0.85 | 2.07 | 2.865 (6) | 156 |
O19—H19A···O13x | 0.85 | 2.12 | 2.661 (8) | 121 |
O19—H19B···O4xi | 0.85 | 2.51 | 3.289 (9) | 152 |
C6—H6···O8iii | 0.98 | 2.43 | 3.370 (7) | 160 |
C7—H7C···O2xii | 0.96 | 2.58 | 3.311 (8) | 134 |
C10—H10···O6v | 0.93 | 2.50 | 3.053 (7) | 118 |
C16—H16···O15 | 0.98 | 2.38 | 2.784 (7) | 104 |
C17—H17C···O13xiii | 0.96 | 2.50 | 3.445 (8) | 166 |
C20—H20C···O19 | 0.96 | 2.48 | 3.396 (9) | 160 |
Symmetry codes: (ii) −x+2, y−1/2, −z+1; (iii) −x, y+1/2, −z+1; (iv) −x+2, y+1/2, −z+1; (v) x+1, y, z; (vi) x−1, y, z; (vii) x+1, y, z+1; (viii) −x+1, y+1/2, −z+2; (ix) x+2, y, z+1; (x) −x+1, y−1/2, −z+1; (xi) −x+1, y−1/2, −z+2; (xii) x, y, z+1; (xiii) x−2, y, z. |
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