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In the title dimeric structure, [K2(C16H23NO8)2{CrClO3}2], the two macrocyclic ligands are oriented head-to-head with the stacked nitrobenzene groups.
Supporting information
CCDC reference: 618270
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.006 Å
- R factor = 0.048
- wR factor = 0.114
- Data-to-parameter ratio = 13.3
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
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
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.29
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C16 H23 Cl1 Cr1 K1 N1 O11
Atom count from _chemical_formula_moiety:C16 H23 Cl1 Cr1 N1 O10
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 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
0 ALERT type 4 Improvement, methodology, query or suggestion
checkCIF publication errors
Alert level A
PUBL024_ALERT_1_A The number of authors is greater than 5.
Please specify the role of each of the co-authors
for your paper.
| Author Response: All authors made significant contribution
in this work. The idea of synthesis belongs to Kamalov and
Kotlyar. The synthesis was performed by Chuprin, Pluzhnik-Gladyr and Kiriyak.
X-ray diffraction experiment was performed by Shishkina.
The analysis of diffraction data was performed by Shishkin.
|
1 ALERT level A = Data missing that is essential or data in wrong format
0 ALERT level G = General alerts. Data that may be required is missing
Data collection: CrysAlis CCD (Oxford Diffraction, 2006); cell refinement: CrysAlis RED (Oxford Diffraction, 2006); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXTL/PC (Sheldrick, 1998); program(s) used to refine structure: SHELXTL/PC; molecular graphics: XP (Siemens, 1998); software used to prepare material for publication: SHELXTL/PC.
bis[(18-nitro-2,3,5,6,8,9,11,12,14,15-
decahydro-1,4,7,10,13,16-benzohexaoxacyclooctadecine)potassium chlorochromate]
top
Crystal data top
[K(C16H23NO8)][CrClO3] | Z = 2 |
Mr = 531.91 | F(000) = 548 |
Triclinic, P1 | Dx = 1.619 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.778 (1) Å | Cell parameters from 3015 reflections |
b = 9.531 (1) Å | θ = 3–34° |
c = 13.678 (1) Å | µ = 0.90 mm−1 |
α = 100.959 (9)° | T = 100 K |
β = 98.728 (9)° | Transparent, yellow |
γ = 98.782 (9)° | 0.20 × 0.20 × 0.10 mm |
V = 1090.8 (2) Å3 | |
Data collection top
Oxford Xcalibur3 diffractometer | 2363 reflections with I > 2σ(I) |
Radiation source: Enhance (Mo) X-ray Source | Rint = 0.039 |
Graphite monochromator | θmax = 25.0°, θmin = 2.9° |
Detector resolution: 16.1827 pixels mm-1 | h = −10→10 |
ω scans | k = −11→11 |
8636 measured reflections | l = −16→16 |
3715 independent reflections | |
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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.114 | H-atom parameters constrained |
S = 0.89 | w = 1/[σ2(Fo2) + (0.0655P)2] where P = (Fo2 + 2Fc2)/3 |
3715 reflections | (Δ/σ)max = 0.001 |
280 parameters | Δρmax = 0.66 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.63954 (11) | 0.80020 (10) | 0.73468 (7) | 0.0284 (2) | |
Cr1 | 0.87776 (8) | 1.14912 (7) | 0.76445 (5) | 0.0299 (2) | |
Cl1 | 0.99518 (14) | 1.16995 (13) | 0.63648 (9) | 0.0419 (3) | |
N1 | 0.5977 (5) | 0.5360 (4) | 1.1852 (3) | 0.0320 (8) | |
O1 | 0.7515 (3) | 0.8150 (3) | 0.9387 (2) | 0.0288 (7) | |
O2 | 0.8963 (3) | 0.6727 (3) | 0.7816 (2) | 0.0302 (7) | |
O3 | 0.7404 (3) | 0.6278 (3) | 0.5796 (2) | 0.0331 (7) | |
O4 | 0.5211 (3) | 0.8019 (3) | 0.5390 (2) | 0.0331 (7) | |
O5 | 0.3398 (3) | 0.8597 (3) | 0.6927 (2) | 0.0293 (7) | |
O6 | 0.4710 (3) | 0.8604 (3) | 0.8962 (2) | 0.0268 (6) | |
O7 | 0.4908 (4) | 0.4894 (3) | 1.2259 (2) | 0.0363 (7) | |
O8 | 0.7294 (4) | 0.5066 (3) | 1.2004 (2) | 0.0412 (8) | |
O9 | 0.9391 (4) | 1.0241 (3) | 0.8127 (2) | 0.0405 (8) | |
O10 | 0.9222 (3) | 1.3011 (3) | 0.8451 (2) | 0.0350 (7) | |
O11 | 0.6933 (3) | 1.1058 (3) | 0.7239 (2) | 0.0383 (8) | |
C1 | 0.4956 (5) | 0.7879 (4) | 0.9720 (3) | 0.0261 (9) | |
C2 | 0.3851 (5) | 0.7465 (4) | 1.0280 (3) | 0.0271 (9) | |
H2 | 0.2848 | 0.7728 | 1.0168 | 0.033* | |
C3 | 0.4197 (5) | 0.6669 (4) | 1.1002 (3) | 0.0280 (10) | |
H3 | 0.3439 | 0.6382 | 1.1388 | 0.034* | |
C4 | 0.5642 (5) | 0.6300 (4) | 1.1153 (3) | 0.0242 (9) | |
C5 | 0.6825 (5) | 0.6762 (4) | 1.0641 (3) | 0.0277 (10) | |
H5 | 0.7838 | 0.6527 | 1.0779 | 0.033* | |
C6 | 0.6471 (5) | 0.7571 (4) | 0.9929 (3) | 0.0253 (9) | |
C7 | 0.9091 (5) | 0.7894 (5) | 0.9535 (3) | 0.0321 (10) | |
H7B | 0.9424 | 0.7827 | 1.0247 | 0.039* | |
H7A | 0.9804 | 0.8718 | 0.9402 | 0.039* | |
C8 | 0.9204 (5) | 0.6493 (5) | 0.8828 (3) | 0.0326 (10) | |
H8B | 1.0250 | 0.6241 | 0.9003 | 0.039* | |
H8A | 0.8396 | 0.5684 | 0.8889 | 0.039* | |
C9 | 0.9010 (5) | 0.5493 (5) | 0.7069 (3) | 0.0357 (11) | |
H9B | 0.8124 | 0.4699 | 0.7043 | 0.043* | |
H9A | 1.0003 | 0.5140 | 0.7229 | 0.043* | |
C10 | 0.8895 (5) | 0.5938 (5) | 0.6072 (4) | 0.0421 (12) | |
H10B | 0.9719 | 0.6797 | 0.6125 | 0.050* | |
H10A | 0.9061 | 0.5136 | 0.5546 | 0.050* | |
C11 | 0.7231 (6) | 0.6831 (5) | 0.4895 (3) | 0.0389 (12) | |
H11B | 0.7525 | 0.6158 | 0.4340 | 0.047* | |
H11A | 0.7931 | 0.7789 | 0.5011 | 0.047* | |
C12 | 0.5578 (6) | 0.6983 (5) | 0.4609 (3) | 0.0376 (12) | |
H12B | 0.5427 | 0.7310 | 0.3962 | 0.045* | |
H12A | 0.4873 | 0.6033 | 0.4517 | 0.045* | |
C13 | 0.3624 (5) | 0.8183 (5) | 0.5186 (3) | 0.0390 (12) | |
H13B | 0.2922 | 0.7231 | 0.5092 | 0.047* | |
H13A | 0.3419 | 0.8544 | 0.4554 | 0.047* | |
C14 | 0.3309 (5) | 0.9231 (5) | 0.6047 (3) | 0.0351 (11) | |
H14B | 0.4092 | 1.0145 | 0.6192 | 0.042* | |
H14A | 0.2253 | 0.9463 | 0.5873 | 0.042* | |
C15 | 0.3098 (5) | 0.9542 (5) | 0.7770 (3) | 0.0317 (10) | |
H15B | 0.2060 | 0.9810 | 0.7601 | 0.038* | |
H15A | 0.3905 | 1.0442 | 0.7957 | 0.038* | |
C16 | 0.3126 (5) | 0.8795 (5) | 0.8637 (3) | 0.0285 (10) | |
H16B | 0.2768 | 0.9387 | 0.9204 | 0.034* | |
H16A | 0.2412 | 0.7837 | 0.8424 | 0.034* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.0350 (6) | 0.0322 (5) | 0.0223 (5) | 0.0152 (4) | 0.0061 (4) | 0.0088 (4) |
Cr1 | 0.0322 (4) | 0.0297 (4) | 0.0310 (4) | 0.0085 (3) | 0.0071 (3) | 0.0113 (3) |
Cl1 | 0.0405 (7) | 0.0553 (8) | 0.0394 (7) | 0.0147 (6) | 0.0181 (5) | 0.0208 (6) |
N1 | 0.042 (2) | 0.027 (2) | 0.026 (2) | 0.0074 (18) | 0.0064 (18) | 0.0032 (16) |
O1 | 0.0302 (17) | 0.0358 (17) | 0.0263 (16) | 0.0127 (13) | 0.0088 (13) | 0.0135 (13) |
O2 | 0.0349 (17) | 0.0263 (16) | 0.0322 (18) | 0.0125 (13) | 0.0092 (13) | 0.0054 (14) |
O3 | 0.0391 (18) | 0.0373 (18) | 0.0264 (17) | 0.0092 (14) | 0.0117 (13) | 0.0096 (14) |
O4 | 0.0413 (19) | 0.0338 (17) | 0.0256 (17) | 0.0091 (14) | 0.0034 (14) | 0.0104 (14) |
O5 | 0.0392 (18) | 0.0266 (16) | 0.0239 (17) | 0.0124 (13) | 0.0028 (13) | 0.0077 (13) |
O6 | 0.0274 (16) | 0.0292 (16) | 0.0250 (16) | 0.0081 (12) | 0.0030 (12) | 0.0084 (13) |
O7 | 0.049 (2) | 0.0343 (18) | 0.0300 (18) | 0.0099 (15) | 0.0128 (15) | 0.0110 (14) |
O8 | 0.036 (2) | 0.044 (2) | 0.047 (2) | 0.0130 (15) | −0.0005 (15) | 0.0209 (16) |
O9 | 0.049 (2) | 0.0350 (18) | 0.043 (2) | 0.0116 (15) | 0.0126 (15) | 0.0136 (15) |
O10 | 0.0396 (19) | 0.0289 (17) | 0.0394 (19) | 0.0076 (13) | 0.0081 (14) | 0.0130 (14) |
O11 | 0.0365 (19) | 0.0447 (19) | 0.0336 (18) | 0.0075 (15) | 0.0059 (14) | 0.0085 (15) |
C1 | 0.033 (3) | 0.020 (2) | 0.024 (2) | 0.0058 (18) | 0.0046 (19) | 0.0016 (18) |
C2 | 0.027 (2) | 0.028 (2) | 0.026 (2) | 0.0062 (18) | 0.0061 (19) | 0.0043 (19) |
C3 | 0.036 (3) | 0.022 (2) | 0.024 (2) | 0.0063 (19) | 0.0047 (19) | 0.0008 (18) |
C4 | 0.040 (3) | 0.018 (2) | 0.013 (2) | 0.0052 (18) | 0.0000 (18) | 0.0008 (17) |
C5 | 0.033 (3) | 0.025 (2) | 0.025 (2) | 0.0093 (19) | 0.0033 (19) | 0.0010 (18) |
C6 | 0.034 (3) | 0.022 (2) | 0.019 (2) | 0.0041 (18) | 0.0035 (18) | 0.0049 (18) |
C7 | 0.027 (3) | 0.044 (3) | 0.029 (3) | 0.010 (2) | 0.0056 (19) | 0.015 (2) |
C8 | 0.029 (2) | 0.031 (3) | 0.039 (3) | 0.0077 (19) | 0.001 (2) | 0.014 (2) |
C9 | 0.036 (3) | 0.035 (3) | 0.039 (3) | 0.014 (2) | 0.009 (2) | 0.007 (2) |
C10 | 0.036 (3) | 0.046 (3) | 0.045 (3) | 0.010 (2) | 0.019 (2) | 0.000 (2) |
C11 | 0.062 (3) | 0.031 (3) | 0.027 (3) | 0.004 (2) | 0.021 (2) | 0.007 (2) |
C12 | 0.065 (4) | 0.030 (3) | 0.019 (2) | 0.005 (2) | 0.009 (2) | 0.010 (2) |
C13 | 0.048 (3) | 0.043 (3) | 0.023 (3) | 0.003 (2) | −0.004 (2) | 0.012 (2) |
C14 | 0.036 (3) | 0.037 (3) | 0.036 (3) | 0.012 (2) | 0.001 (2) | 0.018 (2) |
C15 | 0.032 (3) | 0.030 (2) | 0.035 (3) | 0.0120 (19) | 0.004 (2) | 0.008 (2) |
C16 | 0.026 (2) | 0.033 (2) | 0.028 (2) | 0.0117 (19) | 0.0072 (19) | 0.0023 (19) |
Geometric parameters (Å, º) top
K1—O4 | 2.725 (3) | C2—H2 | 0.9500 |
K1—O2 | 2.768 (3) | C3—C4 | 1.363 (6) |
K1—O3 | 2.769 (3) | C3—H3 | 0.9500 |
K1—O5 | 2.773 (3) | C4—C5 | 1.400 (6) |
K1—O1 | 2.784 (3) | C5—C6 | 1.381 (5) |
K1—O6 | 2.858 (3) | C5—H5 | 0.9500 |
K1—O11 | 2.914 (3) | C7—C8 | 1.518 (6) |
K1—O7i | 3.001 (3) | C7—H7B | 0.9900 |
K1—O9 | 3.029 (3) | C7—H7A | 0.9900 |
Cr1—O9 | 1.591 (3) | C8—H8B | 0.9900 |
Cr1—O11 | 1.593 (3) | C8—H8A | 0.9900 |
Cr1—O10 | 1.599 (3) | C9—C10 | 1.497 (6) |
Cr1—Cl1 | 2.1871 (13) | C9—H9B | 0.9900 |
N1—O8 | 1.228 (4) | C9—H9A | 0.9900 |
N1—O7 | 1.230 (4) | C10—H10B | 0.9900 |
N1—C4 | 1.458 (5) | C10—H10A | 0.9900 |
O1—C6 | 1.378 (5) | C11—C12 | 1.481 (6) |
O1—C7 | 1.432 (5) | C11—H11B | 0.9900 |
O2—C9 | 1.415 (5) | C11—H11A | 0.9900 |
O2—C8 | 1.433 (5) | C12—H12B | 0.9900 |
O3—C10 | 1.410 (5) | C12—H12A | 0.9900 |
O3—C11 | 1.427 (5) | C13—C14 | 1.483 (6) |
O4—C13 | 1.416 (5) | C13—H13B | 0.9900 |
O4—C12 | 1.421 (5) | C13—H13A | 0.9900 |
O5—C15 | 1.407 (5) | C14—H14B | 0.9900 |
O5—C14 | 1.443 (5) | C14—H14A | 0.9900 |
O6—C1 | 1.359 (5) | C15—C16 | 1.494 (6) |
O6—C16 | 1.444 (5) | C15—H15B | 0.9900 |
O7—K1i | 3.001 (3) | C15—H15A | 0.9900 |
C1—C2 | 1.381 (5) | C16—H16B | 0.9900 |
C1—C6 | 1.404 (6) | C16—H16A | 0.9900 |
C2—C3 | 1.381 (6) | | |
| | | |
O4—K1—O2 | 121.00 (9) | C4—C3—C2 | 119.1 (4) |
O4—K1—O3 | 60.97 (9) | C4—C3—H3 | 120.5 |
O2—K1—O3 | 61.06 (8) | C2—C3—H3 | 120.5 |
O4—K1—O5 | 62.31 (9) | C3—C4—C5 | 122.5 (4) |
O2—K1—O5 | 165.09 (9) | C3—C4—N1 | 119.5 (4) |
O3—K1—O5 | 117.09 (9) | C5—C4—N1 | 117.9 (4) |
O4—K1—O1 | 176.09 (9) | C6—C5—C4 | 117.8 (4) |
O2—K1—O1 | 62.59 (8) | C6—C5—H5 | 121.1 |
O3—K1—O1 | 122.85 (9) | C4—C5—H5 | 121.1 |
O5—K1—O1 | 114.68 (8) | O1—C6—C5 | 125.0 (4) |
O4—K1—O6 | 122.98 (9) | O1—C6—C1 | 114.8 (3) |
O2—K1—O6 | 114.30 (8) | C5—C6—C1 | 120.2 (4) |
O3—K1—O6 | 156.13 (9) | O1—C7—C8 | 110.5 (3) |
O5—K1—O6 | 60.67 (8) | O1—C7—H7B | 109.6 |
O1—K1—O6 | 54.04 (8) | C8—C7—H7B | 109.6 |
O4—K1—O11 | 74.94 (9) | O1—C7—H7A | 109.6 |
O2—K1—O11 | 118.68 (9) | C8—C7—H7A | 109.6 |
O3—K1—O11 | 112.07 (9) | H7B—C7—H7A | 108.1 |
O5—K1—O11 | 76.11 (8) | O2—C8—C7 | 107.5 (3) |
O1—K1—O11 | 102.12 (9) | O2—C8—H8B | 110.2 |
O6—K1—O11 | 90.92 (8) | C7—C8—H8B | 110.2 |
O4—K1—O7i | 107.94 (9) | O2—C8—H8A | 110.2 |
O2—K1—O7i | 74.30 (8) | C7—C8—H8A | 110.2 |
O3—K1—O7i | 82.52 (8) | H8B—C8—H8A | 108.5 |
O5—K1—O7i | 90.82 (9) | O2—C9—C10 | 107.6 (3) |
O1—K1—O7i | 74.14 (8) | O2—C9—H9B | 110.2 |
O6—K1—O7i | 73.89 (8) | C10—C9—H9B | 110.2 |
O11—K1—O7i | 163.63 (9) | O2—C9—H9A | 110.2 |
O4—K1—O9 | 110.59 (9) | C10—C9—H9A | 110.2 |
O2—K1—O9 | 68.04 (8) | H9B—C9—H9A | 108.5 |
O3—K1—O9 | 98.04 (9) | O3—C10—C9 | 109.7 (3) |
O5—K1—O9 | 125.83 (9) | O3—C10—H10B | 109.7 |
O1—K1—O9 | 68.78 (8) | C9—C10—H10B | 109.7 |
O6—K1—O9 | 101.40 (8) | O3—C10—H10A | 109.7 |
O11—K1—O9 | 52.06 (8) | C9—C10—H10A | 109.7 |
O7i—K1—O9 | 135.93 (9) | H10B—C10—H10A | 108.2 |
O9—Cr1—O11 | 110.15 (16) | O3—C11—C12 | 109.1 (3) |
O9—Cr1—O10 | 110.65 (16) | O3—C11—H11B | 109.9 |
O11—Cr1—O10 | 111.07 (15) | C12—C11—H11B | 109.9 |
O9—Cr1—Cl1 | 107.50 (12) | O3—C11—H11A | 109.9 |
O11—Cr1—Cl1 | 108.87 (11) | C12—C11—H11A | 109.9 |
O10—Cr1—Cl1 | 108.51 (11) | H11B—C11—H11A | 108.3 |
O8—N1—O7 | 123.2 (4) | O4—C12—C11 | 108.8 (4) |
O8—N1—C4 | 119.1 (4) | O4—C12—H12B | 109.9 |
O7—N1—C4 | 117.7 (4) | C11—C12—H12B | 109.9 |
C6—O1—C7 | 119.5 (3) | O4—C12—H12A | 109.9 |
C6—O1—K1 | 117.0 (2) | C11—C12—H12A | 109.9 |
C7—O1—K1 | 110.6 (2) | H12B—C12—H12A | 108.3 |
C9—O2—C8 | 113.7 (3) | O4—C13—C14 | 109.1 (3) |
C9—O2—K1 | 113.0 (2) | O4—C13—H13B | 109.9 |
C8—O2—K1 | 113.9 (2) | C14—C13—H13B | 109.9 |
C10—O3—C11 | 113.7 (3) | O4—C13—H13A | 109.9 |
C10—O3—K1 | 114.5 (2) | C14—C13—H13A | 109.9 |
C11—O3—K1 | 111.5 (2) | H13B—C13—H13A | 108.3 |
C13—O4—C12 | 112.0 (3) | O5—C14—C13 | 109.0 (3) |
C13—O4—K1 | 116.1 (2) | O5—C14—H14B | 109.9 |
C12—O4—K1 | 117.9 (2) | C13—C14—H14B | 109.9 |
C15—O5—C14 | 111.6 (3) | O5—C14—H14A | 109.9 |
C15—O5—K1 | 110.0 (2) | C13—C14—H14A | 109.9 |
C14—O5—K1 | 107.4 (2) | H14B—C14—H14A | 108.3 |
C1—O6—C16 | 117.3 (3) | O5—C15—C16 | 109.0 (3) |
C1—O6—K1 | 116.5 (2) | O5—C15—H15B | 109.9 |
C16—O6—K1 | 114.0 (2) | C16—C15—H15B | 109.9 |
N1—O7—K1i | 135.6 (2) | O5—C15—H15A | 109.9 |
Cr1—O9—K1 | 95.90 (13) | C16—C15—H15A | 109.9 |
Cr1—O11—K1 | 100.39 (13) | H15B—C15—H15A | 108.3 |
O6—C1—C2 | 124.9 (4) | O6—C16—C15 | 108.7 (3) |
O6—C1—C6 | 115.2 (3) | O6—C16—H16B | 109.9 |
C2—C1—C6 | 119.9 (4) | C15—C16—H16B | 109.9 |
C1—C2—C3 | 120.3 (4) | O6—C16—H16A | 109.9 |
C1—C2—H2 | 119.9 | C15—C16—H16A | 109.9 |
C3—C2—H2 | 119.9 | H16B—C16—H16A | 108.3 |
| | | |
O2—K1—O1—C6 | −122.5 (3) | O9—K1—O6—C1 | −89.3 (3) |
O3—K1—O1—C6 | −112.1 (2) | O4—K1—O6—C16 | 5.0 (3) |
O5—K1—O1—C6 | 41.2 (3) | O2—K1—O6—C16 | −160.1 (2) |
O6—K1—O1—C6 | 39.1 (2) | O3—K1—O6—C16 | −87.1 (3) |
O11—K1—O1—C6 | 121.3 (2) | O5—K1—O6—C16 | 4.1 (2) |
O7i—K1—O1—C6 | −42.3 (2) | O1—K1—O6—C16 | −178.0 (3) |
O9—K1—O1—C6 | 162.0 (3) | O11—K1—O6—C16 | 77.6 (2) |
O2—K1—O1—C7 | 19.0 (2) | O7i—K1—O6—C16 | −96.2 (2) |
O3—K1—O1—C7 | 29.4 (3) | O9—K1—O6—C16 | 129.0 (2) |
O5—K1—O1—C7 | −177.3 (2) | O8—N1—O7—K1i | −45.1 (6) |
O6—K1—O1—C7 | −179.4 (3) | C4—N1—O7—K1i | 134.6 (3) |
O11—K1—O1—C7 | −97.2 (2) | O11—Cr1—O9—K1 | 11.39 (16) |
O7i—K1—O1—C7 | 99.2 (2) | O10—Cr1—O9—K1 | 134.58 (13) |
O9—K1—O1—C7 | −56.5 (2) | Cl1—Cr1—O9—K1 | −107.10 (8) |
O4—K1—O2—C9 | −33.9 (3) | O4—K1—O9—Cr1 | 42.46 (15) |
O3—K1—O2—C9 | −22.2 (2) | O2—K1—O9—Cr1 | 158.67 (15) |
O5—K1—O2—C9 | 64.7 (4) | O3—K1—O9—Cr1 | 104.39 (13) |
O1—K1—O2—C9 | 147.9 (3) | O5—K1—O9—Cr1 | −27.61 (18) |
O6—K1—O2—C9 | 131.6 (2) | O1—K1—O9—Cr1 | −133.41 (15) |
O11—K1—O2—C9 | −122.9 (2) | O6—K1—O9—Cr1 | −89.53 (13) |
O7i—K1—O2—C9 | 67.9 (2) | O11—K1—O9—Cr1 | −7.38 (11) |
O9—K1—O2—C9 | −135.4 (3) | O7i—K1—O9—Cr1 | −168.08 (11) |
O4—K1—O2—C8 | −165.6 (2) | O9—Cr1—O11—K1 | −11.98 (17) |
O3—K1—O2—C8 | −153.9 (3) | O10—Cr1—O11—K1 | −134.92 (12) |
O5—K1—O2—C8 | −67.0 (4) | Cl1—Cr1—O11—K1 | 105.66 (9) |
O1—K1—O2—C8 | 16.2 (2) | O4—K1—O11—Cr1 | −124.74 (14) |
O6—K1—O2—C8 | −0.1 (3) | O2—K1—O11—Cr1 | −7.31 (17) |
O11—K1—O2—C8 | 105.3 (2) | O3—K1—O11—Cr1 | −75.38 (15) |
O7i—K1—O2—C8 | −63.8 (2) | O5—K1—O11—Cr1 | 170.67 (15) |
O9—K1—O2—C8 | 92.8 (2) | O1—K1—O11—Cr1 | 57.91 (14) |
O4—K1—O3—C10 | 155.5 (3) | O6—K1—O11—Cr1 | 111.24 (13) |
O2—K1—O3—C10 | −13.0 (3) | O7i—K1—O11—Cr1 | 132.8 (3) |
O5—K1—O3—C10 | −176.2 (3) | O9—K1—O11—Cr1 | 7.46 (11) |
O1—K1—O3—C10 | −23.5 (3) | C16—O6—C1—C2 | −8.0 (6) |
O6—K1—O3—C10 | −98.0 (3) | K1—O6—C1—C2 | −148.4 (3) |
O11—K1—O3—C10 | 98.5 (3) | C16—O6—C1—C6 | 172.8 (3) |
O7i—K1—O3—C10 | −89.2 (3) | K1—O6—C1—C6 | 32.4 (4) |
O9—K1—O3—C10 | 46.3 (3) | O6—C1—C2—C3 | 176.9 (4) |
O4—K1—O3—C11 | 24.6 (3) | C6—C1—C2—C3 | −4.0 (6) |
O2—K1—O3—C11 | −143.9 (3) | C1—C2—C3—C4 | 0.0 (6) |
O5—K1—O3—C11 | 52.9 (3) | C2—C3—C4—C5 | 3.4 (6) |
O1—K1—O3—C11 | −154.4 (3) | C2—C3—C4—N1 | −174.9 (4) |
O6—K1—O3—C11 | 131.1 (3) | O8—N1—C4—C3 | −178.1 (4) |
O11—K1—O3—C11 | −32.3 (3) | O7—N1—C4—C3 | 2.2 (5) |
O7i—K1—O3—C11 | 140.0 (3) | O8—N1—C4—C5 | 3.5 (5) |
O9—K1—O3—C11 | −84.5 (3) | O7—N1—C4—C5 | −176.2 (3) |
O2—K1—O4—C13 | 157.3 (2) | C3—C4—C5—C6 | −2.7 (6) |
O3—K1—O4—C13 | 145.5 (3) | N1—C4—C5—C6 | 175.7 (3) |
O5—K1—O4—C13 | −6.0 (2) | C7—O1—C6—C5 | 1.5 (6) |
O6—K1—O4—C13 | −6.9 (3) | K1—O1—C6—C5 | 139.4 (3) |
O11—K1—O4—C13 | −88.0 (3) | C7—O1—C6—C1 | −179.5 (3) |
O7i—K1—O4—C13 | 75.2 (3) | K1—O1—C6—C1 | −41.6 (4) |
O9—K1—O4—C13 | −126.6 (3) | C4—C5—C6—O1 | 177.5 (4) |
O2—K1—O4—C12 | 20.2 (3) | C4—C5—C6—C1 | −1.4 (6) |
O3—K1—O4—C12 | 8.5 (3) | O6—C1—C6—O1 | 4.9 (5) |
O5—K1—O4—C12 | −143.1 (3) | C2—C1—C6—O1 | −174.3 (3) |
O6—K1—O4—C12 | −144.0 (3) | O6—C1—C6—C5 | −176.1 (3) |
O11—K1—O4—C12 | 134.9 (3) | C2—C1—C6—C5 | 4.7 (6) |
O7i—K1—O4—C12 | −61.9 (3) | C6—O1—C7—C8 | 88.2 (4) |
O9—K1—O4—C12 | 96.3 (3) | K1—O1—C7—C8 | −52.2 (4) |
O4—K1—O5—C15 | −149.0 (3) | C9—O2—C8—C7 | −178.9 (3) |
O2—K1—O5—C15 | 104.1 (4) | K1—O2—C8—C7 | −47.5 (4) |
O3—K1—O5—C15 | −176.9 (2) | O1—C7—C8—O2 | 68.5 (4) |
O1—K1—O5—C15 | 28.2 (2) | C8—O2—C9—C10 | −174.7 (3) |
O6—K1—O5—C15 | 30.1 (2) | K1—O2—C9—C10 | 53.5 (4) |
O11—K1—O5—C15 | −69.0 (2) | C11—O3—C10—C9 | 175.1 (4) |
O7i—K1—O5—C15 | 101.1 (2) | K1—O3—C10—C9 | 45.3 (4) |
O9—K1—O5—C15 | −52.6 (3) | O2—C9—C10—O3 | −66.6 (5) |
O4—K1—O5—C14 | −27.3 (2) | C10—O3—C11—C12 | 173.3 (4) |
O2—K1—O5—C14 | −134.2 (4) | K1—O3—C11—C12 | −55.4 (4) |
O3—K1—O5—C14 | −55.2 (3) | C13—O4—C12—C11 | −177.8 (3) |
O1—K1—O5—C14 | 149.9 (2) | K1—O4—C12—C11 | −39.1 (4) |
O6—K1—O5—C14 | 151.8 (3) | O3—C11—C12—O4 | 63.0 (4) |
O11—K1—O5—C14 | 52.7 (2) | C12—O4—C13—C14 | 177.8 (3) |
O7i—K1—O5—C14 | −137.2 (2) | K1—O4—C13—C14 | 38.3 (4) |
O9—K1—O5—C14 | 69.1 (3) | C15—O5—C14—C13 | −179.6 (4) |
O4—K1—O6—C1 | 146.7 (2) | K1—O5—C14—C13 | 59.7 (4) |
O2—K1—O6—C1 | −18.5 (3) | O4—C13—C14—O5 | −67.5 (4) |
O3—K1—O6—C1 | 54.6 (3) | C14—O5—C15—C16 | 177.1 (3) |
O5—K1—O6—C1 | 145.8 (3) | K1—O5—C15—C16 | −63.7 (3) |
O1—K1—O6—C1 | −36.4 (2) | C1—O6—C16—C15 | −177.1 (3) |
O11—K1—O6—C1 | −140.7 (3) | K1—O6—C16—C15 | −35.7 (4) |
O7i—K1—O6—C1 | 45.5 (2) | O5—C15—C16—O6 | 67.7 (4) |
Symmetry code: (i) −x+1, −y+1, −z+2. |
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