In the crystal structure of the title compound, [Zn{K(C30H30N20O10)(H2O)}Cl(H2O)][ZnCl4]·5H2O, the [(H2O)3ClZn]+ cation links adjacent [(C30H30N20O10)(H2O)K]+ cations into a polycationic chain. The chain is surrounded by water molecules and disordered [ZnCl4]2− anions and they interact to form a hydrogen-bonded layer structure. One water molecule is encapsulated by the cryptand. The cryptand and the encapsulated water molecule, as well as the K and Zn atoms, one coordinated water molecule and one free water molecule, lie on special positions of site symmetry m.
Supporting information
CCDC reference: 274328
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.005 Å
- R factor = 0.044
- wR factor = 0.134
- Data-to-parameter ratio = 13.5
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT241_ALERT_2_A Check High Ueq as Compared to Neighbors for Cl3'
PLAT780_ALERT_1_A Coordinates do not Form a Properly Connected Set ?
Alert level B
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Zn2
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Cl3
PLAT420_ALERT_2_B D-H Without Acceptor O3W - H3W1 ... ?
PLAT480_ALERT_4_B Long H...A H-Bond Reported H4# .. O1W .. 3.04 Ang.
PLAT731_ALERT_1_B Bond Calc 0.87(5), Rep 0.860(10) ...... 5.00 su-Rat
O5W -H5W1 1.555 1.555
PLAT731_ALERT_1_B Bond Calc 0.86(5), Rep 0.860(10) ...... 5.00 su-Rat
O5W -H5W2 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.86(5), Rep 0.860(10) ...... 5.00 su-Rat
O5W -H8# 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.86(5), Rep 0.860(10) ...... 5.00 su-Rat
O5W -H8# 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.87(5), Rep 0.860(10) ...... 5.00 su-Rat
O5W -H7# 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.87(5), Rep 0.860(10) ...... 5.00 su-Rat
O5W -H7# 1.555 1.555
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . Zn2
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . Zn2'
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . Cl3
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . Cl4
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . Cl3'
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . Cl4'
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.11
PLAT220_ALERT_2_C Large Non-Solvent Cl Ueq(max)/Ueq(min) ... 2.87 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Cl2'
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for Cl4'
PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc.
PLAT702_ALERT_1_C Angle Calc 70.25(4), Rep 70.30(10), Dev.. 1.25 Sigma
O1 -K1 -O3 1.555 1.555 1.555
PLAT702_ALERT_1_C Angle Calc 70.25(4), Rep 70.30(10), Dev.. 1.25 Sigma
O1 -K1 -O3 1.555 1.555 7.575
PLAT702_ALERT_1_C Angle Calc 100.15(3), Rep 100.20(10), Dev.. 1.67 Sigma
O3 -K1 -CL1 1.555 1.555 1.555
PLAT702_ALERT_1_C Angle Calc 100.15(3), Rep 100.20(10), Dev.. 1.67 Sigma
O3 -K1 -CL1 7.575 1.555 1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O2W -H2W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O4W -H4W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.840(10) ...... 3.00 su-Rat
O4W -H4W2 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 70.25(4), Rep 70.30(10) ...... 2.50 su-Rat
O1 -K1 -O3 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 100.15(3), Rep 100.20(10) ...... 3.33 su-Rat
O3 -K1 -CL1 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 113.17(4), Rep 113.20(10) ...... 2.50 su-Rat
O5 -K1 -CL1 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 108(6), Rep 108(2) ...... 3.00 su-Rat
H5W1 -O5W -H5W2 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.850(10) ...... 3.00 su-Rat
O2W -H2# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O4W -H5# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.840(10) ...... 3.00 su-Rat
O4W -H6# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.82(3), Rep 1.830(10) ...... 3.00 su-Rat
H6# -O5W 1.555 1.555
2 ALERT level A = In general: serious problem
10 ALERT level B = Potentially serious problem
30 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
31 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
8 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly-[[[triaquazinc(II)]-µ-chloro-[aquacucurbit[5]urilpotassium(I)]] tetrachlorozincate(II) pentahydrate]
top
Crystal data top
[ZnKCl(C30H30N20O10)(H2O)4][ZnCl4]·5H2O | F(000) = 2736 |
Mr = 1339.97 | Dx = 1.853 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 7889 reflections |
a = 13.3944 (5) Å | θ = 2.3–28.0° |
b = 13.6063 (6) Å | µ = 1.46 mm−1 |
c = 26.354 (1) Å | T = 295 K |
V = 4803.0 (3) Å3 | Block, colorless |
Z = 4 | 0.40 × 0.22 × 0.15 mm |
Data collection top
Bruker APEX area-detector diffractometer | 5703 independent reflections |
Radiation source: fine-focus sealed tube | 4854 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.028 |
φ and ω scans | θmax = 27.5°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −16→17 |
Tmin = 0.538, Tmax = 0.811 | k = −17→17 |
39547 measured reflections | l = −33→33 |
Refinement top
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)] = 0.044 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.134 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0887P)2 + 2.5416P] where P = (Fo2 + 2Fc2)/3 |
5703 reflections | (Δ/σ)max = 0.001 |
424 parameters | Δρmax = 0.80 e Å−3 |
30 restraints | Δρmin = −0.38 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Zn1 | 0.08381 (3) | 0.7500 | 0.58755 (1) | 0.0327 (1) | |
Zn2 | 0.5266 (3) | 0.2500 | 0.7940 (1) | 0.0403 (5) | 0.50 |
Zn2' | 0.5142 (4) | 0.2500 | 0.7915 (2) | 0.068 (1) | 0.50 |
K1 | 0.47198 (7) | 0.7500 | 0.55046 (3) | 0.0450 (2) | |
Cl1 | 0.21954 (6) | 0.7500 | 0.53205 (3) | 0.0381 (2) | |
Cl2 | 0.6093 (6) | 0.3884 (5) | 0.8147 (3) | 0.075 (2) | 0.50 |
Cl3 | 0.5369 (4) | 0.2500 | 0.7064 (1) | 0.0471 (7) | 0.50 |
Cl4 | 0.3828 (3) | 0.2500 | 0.8394 (2) | 0.0751 (8) | 0.50 |
Cl2' | 0.5974 (6) | 0.3865 (5) | 0.8226 (3) | 0.079 (2) | 0.50 |
Cl3' | 0.5222 (8) | 0.2500 | 0.7067 (3) | 0.135 (3) | 0.50 |
Cl4' | 0.3525 (3) | 0.2500 | 0.8107 (2) | 0.089 (1) | 0.50 |
O1 | 0.4574 (2) | 0.7500 | 0.6515 (1) | 0.053 (1) | |
O2 | 0.8853 (2) | 0.7500 | 0.7302 (1) | 0.060 (1) | |
O3 | 0.4983 (1) | 0.5622 (1) | 0.58681 (7) | 0.042 (1) | |
O4 | 0.9266 (1) | 0.5659 (2) | 0.66046 (8) | 0.049 (1) | |
O5 | 0.5730 (1) | 0.6388 (1) | 0.48063 (7) | 0.040 (1) | |
O6 | 1.0078 (1) | 0.6312 (1) | 0.54782 (7) | 0.036 (1) | |
O1w | −0.0527 (2) | 0.7500 | 0.6261 (1) | 0.053 (1) | |
O2w | 0.1299 (1) | 0.6355 (1) | 0.6344 (1) | 0.044 (1) | |
O3w | 0.7034 (5) | 0.7500 | 0.5892 (3) | 0.141 (2) | |
O4w | 0.2986 (2) | 0.5355 (2) | 0.6219 (1) | 0.067 (1) | |
O5w | 0.3448 (4) | 0.3878 (3) | 0.6844 (2) | 0.130 (2) | |
O6w | 0.4213 (3) | 0.7500 | 0.4177 (2) | 0.092 (2) | |
N1 | 0.7353 (2) | 0.6684 (3) | 0.7388 (1) | 0.060 (1) | |
N2 | 0.5657 (2) | 0.6686 (2) | 0.7047 (1) | 0.053 (1) | |
N3 | 0.5924 (2) | 0.5201 (2) | 0.6567 (1) | 0.051 (1) | |
N4 | 0.7665 (2) | 0.5270 (2) | 0.6856 (1) | 0.056 (1) | |
N5 | 0.6450 (2) | 0.4749 (2) | 0.5807 (1) | 0.044 (1) | |
N6 | 0.8179 (2) | 0.4797 (2) | 0.6093 (1) | 0.045 (1) | |
N7 | 0.7021 (1) | 0.5330 (2) | 0.4994 (1) | 0.039 (1) | |
N8 | 0.8767 (1) | 0.5309 (2) | 0.5267 (1) | 0.037 (1) | |
N9 | 0.7326 (1) | 0.6618 (2) | 0.4506 (1) | 0.038 (1) | |
N10 | 0.9069 (1) | 0.6608 (2) | 0.4787 (1) | 0.036 (1) | |
C1 | 0.5222 (3) | 0.7500 | 0.6837 (1) | 0.049 (1) | |
C2 | 0.5324 (2) | 0.5708 (3) | 0.6941 (1) | 0.058 (1) | |
C3 | 0.6310 (2) | 0.6941 (3) | 0.7465 (1) | 0.060 (1) | |
C4 | 0.7728 (2) | 0.5706 (3) | 0.7357 (1) | 0.066 (1) | |
C5 | 0.7940 (3) | 0.7500 | 0.7352 (1) | 0.055 (1) | |
C6 | 0.6844 (2) | 0.4669 (2) | 0.6670 (1) | 0.055 (1) | |
C7 | 0.5713 (2) | 0.5234 (2) | 0.6061 (1) | 0.039 (1) | |
C8 | 0.7197 (2) | 0.4346 (2) | 0.6140 (1) | 0.050 (1) | |
C9 | 0.8449 (2) | 0.5278 (2) | 0.6524 (1) | 0.046 (1) | |
C10 | 0.6440 (2) | 0.4610 (2) | 0.5265 (1) | 0.041 (1) | |
C11 | 0.6604 (2) | 0.6138 (2) | 0.4775 (1) | 0.035 (1) | |
C12 | 0.8056 (2) | 0.5203 (2) | 0.4851 (1) | 0.038 (1) | |
C13 | 0.8857 (2) | 0.4619 (2) | 0.5684 (1) | 0.044 (1) | |
C14 | 0.9361 (2) | 0.6110 (2) | 0.5206 (1) | 0.031 (1) | |
C15 | 0.9546 (2) | 0.7500 | 0.4614 (1) | 0.036 (1) | |
C16 | 0.8269 (2) | 0.6106 (2) | 0.4516 (1) | 0.037 (1) | |
C17 | 0.7137 (3) | 0.7500 | 0.4223 (1) | 0.040 (1) | |
H1w1 | −0.064 (3) | 0.699 (1) | 0.644 (1) | 0.064* | |
H2w1 | 0.088 (2) | 0.590 (2) | 0.639 (1) | 0.053* | |
H2w2 | 0.187 (1) | 0.610 (2) | 0.629 (1) | 0.053* | |
H3w1 | 0.740 (2) | 0.699 (1) | 0.588 (3) | 0.170* | |
H4w1 | 0.351 (2) | 0.562 (3) | 0.611 (2) | 0.080* | |
H4w2 | 0.312 (3) | 0.487 (2) | 0.641 (1) | 0.080* | |
H5w1 | 0.397 (3) | 0.363 (5) | 0.699 (2) | 0.155* | |
H5w2 | 0.293 (3) | 0.358 (5) | 0.696 (3) | 0.155* | |
H6w1 | 0.459 (2) | 0.6991 (4) | 0.422 (2) | 0.111* | |
H2a | 0.4640 | 0.5735 | 0.6822 | 0.069* | |
H2b | 0.5330 | 0.5332 | 0.7254 | 0.069* | |
H3 | 0.6058 | 0.6680 | 0.7787 | 0.072* | |
H4a | 0.7360 | 0.5296 | 0.7593 | 0.079* | |
H4b | 0.8421 | 0.5707 | 0.7463 | 0.079* | |
H6 | 0.6725 | 0.4102 | 0.6892 | 0.066* | |
H8 | 0.7233 | 0.3629 | 0.6112 | 0.060* | |
H10a | 0.6698 | 0.3960 | 0.5188 | 0.049* | |
H10b | 0.5756 | 0.4637 | 0.5145 | 0.049* | |
H12 | 0.8160 | 0.4588 | 0.4664 | 0.046* | |
H13a | 0.8745 | 0.3961 | 0.5555 | 0.053* | |
H13b | 0.9534 | 0.4646 | 0.5814 | 0.053* | |
H15a | 0.9555 | 0.7500 | 0.4246 | 0.043* | |
H15b | 1.0234 | 0.7500 | 0.4729 | 0.043* | |
H16 | 0.8480 | 0.5912 | 0.4175 | 0.044* | |
H17a | 0.7554 | 0.7500 | 0.3922 | 0.047* | |
H17b | 0.6446 | 0.7500 | 0.4113 | 0.047* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Zn1 | 0.0284 (2) | 0.0358 (2) | 0.0339 (2) | 0.000 | 0.0049 (1) | 0.000 |
Zn2 | 0.052 (1) | 0.028 (1) | 0.041 (1) | 0.000 | 0.001 (1) | 0.000 |
Zn2' | 0.056 (1) | 0.097 (2) | 0.051 (2) | 0.000 | −0.001 (1) | 0.000 |
K1 | 0.0525 (5) | 0.0394 (4) | 0.0432 (4) | 0.000 | 0.0060 (3) | 0.000 |
Cl1 | 0.0323 (4) | 0.0307 (4) | 0.0513 (5) | 0.000 | 0.0141 (3) | 0.000 |
Cl2 | 0.097 (2) | 0.061 (2) | 0.068 (2) | −0.031 (2) | 0.008 (2) | −0.002 (2) |
Cl3 | 0.062 (2) | 0.044 (1) | 0.035 (2) | 0.000 | −0.006 (1) | 0.000 |
Cl4 | 0.066 (2) | 0.070 (2) | 0.090 (2) | 0.000 | 0.027 (2) | 0.000 |
Cl2' | 0.100 (3) | 0.070 (3) | 0.067 (2) | 0.010 (2) | −0.026 (2) | −0.030 (2) |
Cl3' | 0.132 (7) | 0.198 (7) | 0.074 (4) | 0.000 | −0.019 (4) | 0.000 |
Cl4' | 0.055 (2) | 0.099 (2) | 0.113 (3) | 0.000 | 0.025 (2) | 0.000 |
O1 | 0.036 (1) | 0.087 (2) | 0.038 (1) | 0.000 | −0.006 (1) | 0.000 |
O2 | 0.029 (1) | 0.110 (3) | 0.042 (2) | 0.000 | −0.006 (1) | 0.000 |
O3 | 0.031 (1) | 0.043 (1) | 0.052 (1) | 0.004 (1) | 0.001 (1) | 0.004 (1) |
O4 | 0.031 (1) | 0.054 (1) | 0.064 (1) | −0.003 (1) | −0.003 (1) | 0.018 (1) |
O5 | 0.026 (1) | 0.037 (1) | 0.058 (1) | 0.002 (1) | 0.004 (1) | −0.008 (1) |
O6 | 0.027 (1) | 0.033 (1) | 0.048 (1) | −0.004 (1) | −0.002 (1) | −0.004 (1) |
O1w | 0.057 (2) | 0.040 (1) | 0.063 (2) | 0.000 | 0.028 (1) | 0.000 |
O2w | 0.041 (1) | 0.049 (1) | 0.041 (1) | −0.002 (1) | −0.002 (1) | 0.007 (1) |
O3w | 0.146 (6) | 0.143 (6) | 0.135 (5) | 0.000 | −0.012 (5) | 0.000 |
O4w | 0.037 (1) | 0.081 (2) | 0.083 (2) | −0.001 (1) | 0.003 (1) | 0.014 (1) |
O5w | 0.133 (3) | 0.089 (3) | 0.167 (4) | 0.027 (3) | −0.025 (3) | 0.029 (3) |
O6w | 0.058 (2) | 0.066 (2) | 0.153 (5) | 0.000 | −0.021 (2) | 0.000 |
N1 | 0.032 (1) | 0.104 (2) | 0.043 (1) | 0.000 (1) | −0.004 (1) | 0.019 (1) |
N2 | 0.032 (1) | 0.095 (2) | 0.033 (1) | 0.004 (1) | −0.002 (1) | 0.005 (1) |
N3 | 0.031 (1) | 0.067 (2) | 0.056 (1) | −0.002 (1) | 0.002 (1) | 0.024 (1) |
N4 | 0.034 (1) | 0.079 (2) | 0.056 (1) | −0.007 (1) | 0.000 (1) | 0.031 (1) |
N5 | 0.030 (1) | 0.036 (1) | 0.065 (1) | 0.003 (1) | −0.001 (1) | 0.006 (1) |
N6 | 0.028 (1) | 0.040 (1) | 0.068 (2) | −0.005 (1) | 0.000 (1) | 0.016 (1) |
N7 | 0.024 (1) | 0.033 (1) | 0.058 (1) | −0.001 (1) | 0.003 (1) | −0.008 (1) |
N8 | 0.026 (1) | 0.031 (1) | 0.055 (1) | −0.004 (1) | −0.001 (1) | −0.006 (1) |
N9 | 0.027 (1) | 0.041 (1) | 0.045 (1) | −0.001 (1) | 0.002 (1) | −0.007 (1) |
N10 | 0.028 (1) | 0.043 (1) | 0.038 (1) | −0.008 (1) | 0.001 (1) | −0.004 (1) |
C1 | 0.028 (2) | 0.092 (3) | 0.027 (2) | 0.000 | 0.006 (1) | 0.000 |
C2 | 0.028 (1) | 0.103 (3) | 0.042 (1) | −0.010 (1) | 0.006 (1) | 0.023 (2) |
C3 | 0.034 (1) | 0.123 (3) | 0.024 (1) | 0.000 (2) | 0.003 (1) | 0.012 (1) |
C4 | 0.037 (1) | 0.115 (3) | 0.046 (2) | −0.001 (2) | −0.010 (1) | 0.044 (2) |
C5 | 0.036 (2) | 0.105 (4) | 0.022 (2) | 0.000 | −0.008 (1) | 0.000 |
C6 | 0.032 (1) | 0.062 (2) | 0.072 (2) | −0.006 (1) | −0.002 (1) | 0.042 (2) |
C7 | 0.027 (1) | 0.034 (1) | 0.055 (2) | −0.006 (1) | 0.004 (1) | 0.012 (1) |
C8 | 0.029 (1) | 0.032 (1) | 0.089 (2) | −0.004 (1) | −0.002 (1) | 0.025 (1) |
C9 | 0.032 (1) | 0.045 (1) | 0.062 (2) | 0.002 (1) | −0.002 (1) | 0.029 (1) |
C10 | 0.027 (1) | 0.025 (1) | 0.071 (2) | −0.004 (1) | 0.000 (1) | −0.011 (1) |
C11 | 0.030 (1) | 0.032 (1) | 0.042 (1) | −0.004 (1) | 0.001 (1) | −0.016 (1) |
C12 | 0.026 (1) | 0.034 (1) | 0.055 (1) | 0.000 (1) | 0.003 (1) | −0.019 (1) |
C13 | 0.026 (1) | 0.027 (1) | 0.080 (2) | 0.004 (1) | −0.001 (1) | 0.005 (1) |
C14 | 0.022 (1) | 0.029 (1) | 0.041 (1) | 0.001 (1) | 0.007 (1) | −0.009 (1) |
C15 | 0.027 (2) | 0.044 (2) | 0.036 (2) | 0.000 | 0.010 (1) | 0.000 |
C16 | 0.027 (1) | 0.045 (1) | 0.038 (1) | 0.000 (1) | 0.004 (1) | −0.017 (1) |
C17 | 0.036 (2) | 0.056 (2) | 0.027 (2) | 0.000 | −0.003 (1) | 0.000 |
Geometric parameters (Å, º) top
Zn1—O6i | 2.178 (2) | N7—C11 | 1.363 (3) |
Zn1—O6ii | 2.178 (2) | N7—C10 | 1.440 (3) |
Zn1—O1w | 2.092 (3) | N7—C12 | 1.447 (3) |
Zn1—O2w | 2.082 (2) | N8—C14 | 1.359 (3) |
Zn1—O2wiii | 2.082 (2) | N8—C13 | 1.450 (4) |
Zn1—Cl1 | 2.333 (1) | N8—C12 | 1.460 (3) |
Zn2—Cl2 | 2.251 (6) | N9—C11 | 1.366 (3) |
Zn2—Cl2iv | 2.251 (6) | N9—C17 | 1.434 (3) |
Zn2—Cl3 | 2.311 (4) | N9—C16 | 1.442 (3) |
Zn2—Cl4 | 2.268 (5) | N10—C14 | 1.354 (3) |
Zn2'—Cl2' | 2.316 (6) | N10—C15 | 1.446 (3) |
Zn2'—Cl2'iv | 2.316 (6) | N10—C16 | 1.456 (3) |
Zn2'—Cl3' | 2.239 (8) | C1—N2iii | 1.368 (4) |
Zn2'—Cl4' | 2.224 (6) | C3—C3iii | 1.520 (8) |
K1—O1 | 2.669 (3) | C5—N1iii | 1.364 (4) |
K1—O3 | 2.752 (2) | C6—C8 | 1.539 (5) |
K1—O3iii | 2.752 (2) | C12—C16 | 1.539 (4) |
K1—O5 | 2.740 (2) | C15—N10iii | 1.446 (3) |
K1—O5iii | 2.740 (2) | C17—N9iii | 1.434 (3) |
K1—O3w | 3.264 (7) | O1w—H1w1 | 0.85 (1) |
K1—Cl1 | 3.416 (1) | O2w—H2w1 | 0.85 (1) |
O1—C1 | 1.215 (5) | O2w—H2w2 | 0.85 (1) |
O2—C5 | 1.230 (5) | O3w—H3w1 | 0.85 (1) |
O3—C7 | 1.222 (3) | O4w—H4w1 | 0.84 (1) |
O4—C9 | 1.230 (3) | O4w—H4w2 | 0.84 (1) |
O5—C11 | 1.222 (3) | O5w—H5w1 | 0.86 (1) |
O6—C14 | 1.230 (3) | O5w—H5w2 | 0.86 (1) |
N1—C5 | 1.364 (4) | O6w—H6w1 | 0.86 (1) |
N1—C4 | 1.426 (5) | C2—H2a | 0.97 |
N1—C3 | 1.454 (4) | C2—H2b | 0.97 |
N2—C1 | 1.368 (4) | C3—H3 | 0.98 |
N2—C2 | 1.431 (5) | C4—H4a | 0.97 |
N2—C3 | 1.449 (4) | C4—H4b | 0.97 |
N3—C7 | 1.364 (4) | C6—H6 | 0.98 |
N3—C2 | 1.446 (4) | C8—H8 | 0.98 |
N3—C6 | 1.454 (4) | C10—H10a | 0.97 |
N4—C9 | 1.366 (4) | C10—H10b | 0.97 |
N4—C4 | 1.450 (5) | C12—H12 | 0.98 |
N4—C6 | 1.455 (4) | C13—H13a | 0.97 |
N5—C7 | 1.363 (3) | C13—H13b | 0.97 |
N5—C8 | 1.440 (3) | C15—H15a | 0.97 |
N5—C10 | 1.442 (4) | C15—H15b | 0.97 |
N6—C9 | 1.360 (4) | C16—H16 | 0.98 |
N6—C13 | 1.430 (4) | C17—H17a | 0.97 |
N6—C8 | 1.457 (3) | C17—H17b | 0.97 |
| | | |
O6i—Zn1—O6ii | 95.8 (1) | N2—C3—C3iii | 103.9 (2) |
O6i—Zn1—O1w | 79.9 (1) | N1—C3—C3iii | 103.9 (2) |
O6i—Zn1—O2w | 82.4 (1) | N1—C4—N4 | 114.5 (2) |
O6i—Zn1—O2wiii | 168.3 (1) | O2—C5—N1 | 125.5 (2) |
O6i—Zn1—Cl1 | 93.6 (1) | O2—C5—N1iii | 125.5 (2) |
O6ii—Zn1—O2wiii | 82.4 (1) | N1—C5—N1iii | 108.9 (4) |
O6ii—Zn1—O1w | 79.9 (1) | N3—C6—N4 | 115.1 (3) |
O6ii—Zn1—O2w | 168.3 (1) | N3—C6—C8 | 103.5 (2) |
O6ii—Zn1—Cl1 | 93.6 (1) | N4—C6—C8 | 103.5 (2) |
O1w—Zn1—O2w | 88.3 (1) | O3—C7—N5 | 125.7 (3) |
O1w—Zn1—O2wiii | 88.3 (1) | O3—C7—N3 | 125.9 (3) |
O1w—Zn1—Cl1 | 170.3 (1) | N5—C7—N3 | 108.4 (2) |
O2w—Zn1—Cl1 | 98.1 (1) | N5—C8—N6 | 114.6 (2) |
O2w—Zn1—O2wiii | 96.9 (1) | N5—C8—C6 | 103.4 (2) |
O2wiii—Zn1—Cl1 | 98.1 (1) | N6—C8—C6 | 103.6 (2) |
Cl2—Zn2—Cl2iv | 113.5 (5) | O4—C9—N6 | 125.7 (3) |
Cl2—Zn2—Cl3 | 102.3 (2) | O4—C9—N4 | 125.3 (3) |
Cl2—Zn2—Cl4 | 106.8 (2) | N6—C9—N4 | 109.0 (2) |
Cl2iv—Zn2—Cl3 | 102.3 (2) | N7—C10—N5 | 113.4 (2) |
Cl2iv—Zn2—Cl4 | 106.8 (2) | O5—C11—N7 | 126.1 (2) |
Cl3—Zn2—Cl4 | 125.3 (3) | O5—C11—N9 | 125.5 (2) |
Cl2'—Zn2'—Cl2'iv | 106.6 (4) | N7—C11—N9 | 108.4 (2) |
Cl2'—Zn2'—Cl3' | 109.3 (3) | N7—C12—N8 | 114.7 (2) |
Cl2'—Zn2'—Cl4' | 112.8 (3) | N7—C12—C16 | 103.4 (2) |
Cl2'iv—Zn2'—Cl3' | 109.3 (3) | N8—C12—C16 | 103.3 (2) |
Cl2'iv—Zn2'—Cl4' | 112.8 (3) | N6—C13—N8 | 114.2 (2) |
Cl3'—Zn2'—Cl4' | 105.9 (4) | O6—C14—N10 | 126.1 (2) |
O1—K1—O3 | 70.3 (1) | O6—C14—N8 | 124.6 (2) |
O1—K1—O3iii | 70.3 (1) | N10—C14—N8 | 109.2 (2) |
O1—K1—O5 | 134.9 (1) | N10—C15—N10iii | 114.2 (3) |
O1—K1—O5iii | 134.9 (1) | N9—C16—N10 | 115.3 (2) |
O1—K1—O3w | 76.0 (2) | N9—C16—C12 | 103.6 (2) |
O1—K1—Cl1 | 94.0 (1) | N10—C16—C12 | 103.3 (2) |
O3—K1—O3iii | 136.4 (1) | N9iii—C17—N9 | 113.5 (3) |
O3—K1—O5 | 70.0 (1) | Zn1—O1w—H1w1 | 115 (2) |
O3—K1—O5iii | 133.1 (1) | Zn1—O2w—H2w1 | 116 (2) |
O3—K1—O3w | 76.7 (1) | Zn1—O2w—H2w2 | 118 (2) |
O3—K1—Cl1 | 100.2 (1) | H2w1—O2w—H2w2 | 109 (2) |
O3iii—K1—O5 | 133.1 (1) | K1—O3w—H3w1 | 122 (3) |
O3iii—K1—O5iii | 70.0 (1) | H4w1—O4w—H4w2 | 112 (2) |
O3iii—K1—O3w | 76.7 (1) | H5w1—O5w—H5w2 | 108 (2) |
O3iii—K1—Cl1 | 100.2 (1) | N2—C2—H2a | 108.8 |
O5—K1—O5iii | 67.0 (1) | N3—C2—H2a | 108.8 |
O5—K1—O3w | 75.0 (1) | N2—C2—H2b | 108.8 |
O5—K1—Cl1 | 113.2 (1) | N3—C2—H2b | 108.8 |
O5iii—K1—Cl1 | 113.2 (1) | H2a—C2—H2b | 107.7 |
O3w—K1—Cl1 | 169.9 (2) | N2—C3—H3 | 111.3 |
Zn1—Cl1—K1 | 133.02 (4) | N1—C3—H3 | 111.3 |
C1—O1—K1 | 130.2 (2) | C3iii—C3—H3 | 111.3 |
C7—O3—K1 | 130.4 (2) | N1—C4—H4a | 108.6 |
C11—O5—K1 | 132.3 (2) | N4—C4—H4a | 108.6 |
C14—O6—Zn1v | 144.2 (2) | N1—C4—H4b | 108.6 |
C5—N1—C4 | 123.5 (3) | N4—C4—H4b | 108.6 |
C5—N1—C3 | 111.6 (3) | H4a—C4—H4b | 107.6 |
C4—N1—C3 | 124.9 (3) | N3—C6—H6 | 111.4 |
C1—N2—C2 | 122.8 (2) | N4—C6—H6 | 111.4 |
C1—N2—C3 | 111.7 (3) | C8—C6—H6 | 111.4 |
C2—N2—C3 | 124.0 (3) | N5—C8—H8 | 111.6 |
C7—N3—C2 | 122.4 (2) | N6—C8—H8 | 111.6 |
C7—N3—C6 | 112.0 (3) | C6—C8—H8 | 111.6 |
C2—N3—C6 | 125.5 (3) | N7—C10—H10a | 108.9 |
C9—N4—C4 | 122.3 (3) | N5—C10—H10a | 108.9 |
C9—N4—C6 | 111.8 (3) | N7—C10—H10b | 108.9 |
C4—N4—C6 | 125.4 (2) | N5—C10—H10b | 108.9 |
C7—N5—C8 | 112.8 (3) | H10a—C10—H10b | 107.7 |
C7—N5—C10 | 123.0 (2) | N7—C12—H12 | 111.6 |
C8—N5—C10 | 124.1 (2) | N8—C12—H12 | 111.6 |
C9—N6—C13 | 122.8 (2) | C16—C12—H12 | 111.6 |
C9—N6—C8 | 111.8 (2) | N6—C13—H13a | 108.7 |
C13—N6—C8 | 124.5 (3) | N8—C13—H13a | 108.7 |
C11—N7—C10 | 122.5 (2) | N6—C13—H13b | 108.7 |
C11—N7—C12 | 112.2 (2) | N8—C13—H13b | 108.7 |
C10—N7—C12 | 124.4 (2) | H13a—C13—H13b | 107.6 |
C14—N8—C13 | 124.1 (2) | N10—C15—H15a | 108.7 |
C14—N8—C12 | 111.9 (2) | N10iii—C15—H15a | 108.7 |
C13—N8—C12 | 124.0 (2) | N10—C15—H15b | 108.7 |
C11—N9—C17 | 123.0 (2) | N10iii—C15—H15b | 108.7 |
C11—N9—C16 | 112.3 (2) | H15a—C15—H15b | 107.6 |
C17—N9—C16 | 124.7 (2) | N9—C16—H16 | 111.4 |
C14—N10—C15 | 123.4 (2) | N10—C16—H16 | 111.4 |
C14—N10—C16 | 112.2 (2) | C12—C16—H16 | 111.4 |
C15—N10—C16 | 124.4 (2) | N9iii—C17—H17a | 108.9 |
O1—C1—N2iii | 125.9 (2) | N9—C17—H17a | 108.9 |
O1—C1—N2 | 125.9 (2) | N9iii—C17—H17b | 108.9 |
N2iii—C1—N2 | 108.1 (3) | N9—C17—H17b | 108.9 |
N2—C2—N3 | 113.8 (2) | H17a—C17—H17b | 107.7 |
N2—C3—N1 | 114.6 (3) | | |
| | | |
O2wiii—Zn1—Cl1—K1 | 49.10 (6) | C7—N5—C8—N6 | −113.2 (3) |
O2w—Zn1—Cl1—K1 | −49.10 (6) | C10—N5—C8—N6 | 70.2 (3) |
O6i—Zn1—Cl1—K1 | −131.97 (5) | C7—N5—C8—C6 | −1.2 (3) |
O6ii—Zn1—Cl1—K1 | 131.97 (5) | C10—N5—C8—C6 | −177.8 (2) |
O1—K1—Cl1—Zn1 | 0.0 | C9—N6—C8—N5 | 115.0 (3) |
O5—K1—Cl1—Zn1 | 143.09 (5) | C13—N6—C8—N5 | −75.3 (3) |
O5iii—K1—Cl1—Zn1 | −143.09 (5) | C9—N6—C8—C6 | 3.1 (3) |
O3iii—K1—Cl1—Zn1 | −70.63 (4) | C13—N6—C8—C6 | 172.9 (2) |
O3—K1—Cl1—Zn1 | 70.63 (4) | N3—C6—C8—N5 | 1.1 (3) |
O3w—K1—Cl1—Zn1 | 0.0 | N4—C6—C8—N5 | −119.3 (2) |
O5—K1—O1—C1 | 51.24 (8) | N3—C6—C8—N6 | 120.9 (2) |
O5iii—K1—O1—C1 | −51.24 (8) | N4—C6—C8—N6 | 0.5 (3) |
O3iii—K1—O1—C1 | −80.63 (5) | C13—N6—C9—O4 | 4.1 (4) |
O3—K1—O1—C1 | 80.63 (5) | C8—N6—C9—O4 | 174.1 (2) |
O3w—K1—O1—C1 | 0.000 (1) | C13—N6—C9—N4 | −175.7 (2) |
Cl1—K1—O1—C1 | 180.000 (1) | C8—N6—C9—N4 | −5.8 (3) |
O1—K1—O3—C7 | −78.9 (2) | C4—N4—C9—O4 | −1.4 (4) |
O5—K1—O3—C7 | 79.4 (2) | C6—N4—C9—O4 | −173.7 (2) |
O5iii—K1—O3—C7 | 54.8 (3) | C4—N4—C9—N6 | 178.5 (3) |
O3iii—K1—O3—C7 | −52.9 (3) | C6—N4—C9—N6 | 6.2 (3) |
O3w—K1—O3—C7 | 0.7 (3) | C11—N7—C10—N5 | −97.8 (3) |
Cl1—K1—O3—C7 | −169.5 (2) | C12—N7—C10—N5 | 93.2 (3) |
O1—K1—O5—C11 | −50.0 (3) | C7—N5—C10—N7 | 96.6 (3) |
O5iii—K1—O5—C11 | 81.3 (2) | C8—N5—C10—N7 | −87.2 (3) |
O3iii—K1—O5—C11 | 56.2 (3) | K1—O5—C11—N7 | 86.9 (3) |
O3—K1—O5—C11 | −79.4 (2) | K1—O5—C11—N9 | −94.2 (3) |
O3w—K1—O5—C11 | 1.5 (2) | C10—N7—C11—O5 | 5.3 (4) |
Cl1—K1—O5—C11 | −172.2 (2) | C12—N7—C11—O5 | 175.5 (2) |
K1—O1—C1—N2iii | 89.4 (3) | C10—N7—C11—N9 | −173.8 (2) |
K1—O1—C1—N2 | −89.4 (3) | C12—N7—C11—N9 | −3.5 (3) |
C2—N2—C1—O1 | −6.0 (5) | C17—N9—C11—O5 | 0.4 (4) |
C3—N2—C1—O1 | −172.6 (3) | C16—N9—C11—O5 | −176.3 (2) |
C2—N2—C1—N2iii | 175.0 (2) | C17—N9—C11—N7 | 179.5 (2) |
C3—N2—C1—N2iii | 8.4 (4) | C16—N9—C11—N7 | 2.8 (3) |
C1—N2—C2—N3 | 99.6 (3) | C11—N7—C12—N8 | 114.5 (2) |
C3—N2—C2—N3 | −95.4 (3) | C10—N7—C12—N8 | −75.5 (3) |
C7—N3—C2—N2 | −90.6 (3) | C11—N7—C12—C16 | 2.8 (3) |
C6—N3—C2—N2 | 84.5 (3) | C10—N7—C12—C16 | 172.8 (2) |
C1—N2—C3—N1 | −117.8 (3) | C14—N8—C12—N7 | −113.8 (2) |
C2—N2—C3—N1 | 75.8 (4) | C13—N8—C12—N7 | 68.6 (3) |
C1—N2—C3—C3iii | −5.0 (2) | C14—N8—C12—C16 | −2.0 (2) |
C2—N2—C3—C3iii | −171.5 (2) | C13—N8—C12—C16 | −179.6 (2) |
C5—N1—C3—N2 | 113.5 (3) | C9—N6—C13—N8 | −99.1 (3) |
C4—N1—C3—N2 | −66.8 (4) | C8—N6—C13—N8 | 92.3 (3) |
C5—N1—C3—C3iii | 0.8 (2) | C14—N8—C13—N6 | 97.3 (3) |
C4—N1—C3—C3iii | −179.5 (2) | C12—N8—C13—N6 | −85.4 (3) |
C5—N1—C4—N4 | −95.6 (3) | Zn1v—O6—C14—N10 | 47.1 (4) |
C3—N1—C4—N4 | 84.7 (3) | Zn1v—O6—C14—N8 | −136.9 (2) |
C9—N4—C4—N1 | 95.9 (3) | C15—N10—C14—O6 | −3.5 (4) |
C6—N4—C4—N1 | −92.9 (4) | C16—N10—C14—O6 | 172.7 (2) |
C4—N1—C5—O2 | −1.9 (5) | C15—N10—C14—N8 | 180.0 (2) |
C3—N1—C5—O2 | 177.8 (3) | C16—N10—C14—N8 | −3.8 (3) |
C4—N1—C5—N1iii | 178.9 (2) | C13—N8—C14—O6 | 4.6 (4) |
C3—N1—C5—N1iii | −1.4 (4) | C12—N8—C14—O6 | −173.0 (2) |
C7—N3—C6—N4 | 111.5 (3) | C13—N8—C14—N10 | −178.8 (2) |
C2—N3—C6—N4 | −64.0 (4) | C12—N8—C14—N10 | 3.7 (2) |
C7—N3—C6—C8 | −0.6 (3) | C14—N10—C15—N10iii | −94.9 (3) |
C2—N3—C6—C8 | −176.1 (3) | C16—N10—C15—N10iii | 89.4 (3) |
C9—N4—C6—N3 | −116.1 (3) | C11—N9—C16—N10 | −113.2 (2) |
C4—N4—C6—N3 | 71.9 (4) | C17—N9—C16—N10 | 70.3 (3) |
C9—N4—C6—C8 | −4.0 (3) | C11—N9—C16—C12 | −1.0 (2) |
C4—N4—C6—C8 | −176.0 (3) | C17—N9—C16—C12 | −177.6 (2) |
K1—O3—C7—N5 | −89.4 (3) | C14—N10—C16—N9 | 114.7 (2) |
K1—O3—C7—N3 | 91.6 (3) | C15—N10—C16—N9 | −69.2 (3) |
C8—N5—C7—O3 | −178.3 (2) | C14—N10—C16—C12 | 2.4 (2) |
C10—N5—C7—O3 | −1.7 (4) | C15—N10—C16—C12 | 178.6 (2) |
C8—N5—C7—N3 | 0.9 (3) | N7—C12—C16—N9 | −1.0 (2) |
C10—N5—C7—N3 | 177.5 (2) | N8—C12—C16—N9 | −120.8 (2) |
C2—N3—C7—O3 | −5.3 (4) | N7—C12—C16—N10 | 119.6 (2) |
C6—N3—C7—O3 | 179.1 (2) | N8—C12—C16—N10 | −0.2 (2) |
C2—N3—C7—N5 | 175.6 (2) | C11—N9—C17—N9iii | 92.8 (3) |
C6—N3—C7—N5 | −0.1 (3) | C16—N9—C17—N9iii | −90.9 (3) |
Symmetry codes: (i) x−1, y, z; (ii) x−1, −y+3/2, z; (iii) x, −y+3/2, z; (iv) x, −y+1/2, z; (v) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O2i | 0.85 (1) | 2.48 (2) | 2.865 (4) | 109 (1) |
O1w—H1w1···O4i | 0.85 (1) | 1.87 (1) | 2.678 (2) | 159 (2) |
O2w—H2w1···O4i | 0.85 (1) | 2.25 (2) | 2.963 (3) | 141 (2) |
O2w—H2w2···O4w | 0.85 (1) | 1.82 (1) | 2.659 (3) | 169 (3) |
O3w—H3w1···O1wv | 0.85 (1) | 3.04 (4) | 3.408 (8) | 109 (3) |
O4w—H4w1···O3 | 0.84 (1) | 2.08 (2) | 2.853 (3) | 154 (4) |
O4w—H4w2···O5w | 0.84 (1) | 1.83 (1) | 2.672 (5) | 176 (4) |
O5w—H5w2···Cl2vi | 0.86 (1) | 2.52 (5) | 3.16 (1) | 132 (5) |
O5w—H5w2···Cl2′vi | 0.86 (1) | 2.70 (5) | 3.320 (9) | 130 (5) |
O5w—H5w1···Cl3 | 0.86 (1) | 2.43 (4) | 3.236 (6) | 155 (7) |
O5w—H5w1···Cl3′ | 0.86 (1) | 2.29 (4) | 3.083 (9) | 154 (7) |
O6w—H6w1···O5 | 0.86 (1) | 2.32 (3) | 3.028 (4) | 139 (4) |
Symmetry codes: (i) x−1, y, z; (v) x+1, y, z; (vi) x−1/2, y, −z+3/2. |