The title compound, [KCr(C
2O
2)
2(C
6H
8N
2)]
n, was obtained from aqueous solution and analyzed with single-crystal X-ray diffraction at 100 K. It crystallizes in the monoclinic space group
C2/
c and displays a three-dimensional polymeric architecture built up by bimetallic oxalate-bridged Cr
III-K helical chains linked through centrosymmetric K
2O
2 units to yield a sheet-like alternating
P/
M arrangement which looks like that of the previously described two-dimensional [NaCr(ox)
2(pyim)(H
2O)]·2H
2O [pyim is 2-(pyridin-2-yl)imidazole; Lei
et al. (2006).
Inorg. Chem. Commun. 9, 486-488]. The Cr
III ions in each helix have the same chirality. The infinite neutral sheets are eclipsed with respect to each other and are held together by a hydrogen-bonding network involving 2-(aminomethyl)pyridine H atoms and oxalate O atoms. Each sheet gives rise to channels of Cr
4K
4 octanuclear rings and each resultant hole is occupied by a pair of 2-(aminomethyl)pyridine ligands with partial overlap. The shortest Cr
Cr distance [5.593 (4) Å] is shorter than usually observed in the K-
MIII-oxalate family.
Supporting information
CCDC reference: 971307
Data collection: APEX2 (Bruker, 2013); cell refinement: APEX2 (Bruker, 2013); data reduction: CrysAlis PRO (Agilent, 2011) [should this be SAINT (Bruker, 2013)?]; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND for Windows (Brandenburg, 2004) and
Mercury for Windows (Macrae et al.,2006); software used to prepare material for publication: enCIFer (CCDC, 2003).
Poly[[2-(aminomethyl)pyridine]di-µ
6-oxalato-chromium(III)potassium(I)]
top
Crystal data top
[KCr(C2O2)2(C6H8N2)] | F(000) = 1512 |
Mr = 375.28 | Dx = 1.947 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 16.1492 (9) Å | Cell parameters from 24083 reflections |
b = 14.8618 (9) Å | θ = 1.9–37.9° |
c = 13.1617 (11) Å | µ = 1.27 mm−1 |
β = 125.860 (2)° | T = 100 K |
V = 2560.1 (3) Å3 | Prism, pink |
Z = 8 | 0.15 × 0.13 × 0.11 mm |
Data collection top
Bruker D8 Venture Photon diffractometer | 2946 independent reflections |
Radiation source: fine-focus sealed tube | 2509 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.038 |
ω scans | θmax = 27.5°, θmin = 2.1° |
Absorption correction: multi-scan (CrysAlis PRO, Agilent, 2011)
[should this be SADABS (Bruker, 2013)?] | h = −20→20 |
Tmin = 0.812, Tmax = 1 | k = −19→19 |
34973 measured reflections | l = −17→17 |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.091 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0477P)2 + 7.868P] where P = (Fo2 + 2Fc2)/3 |
2946 reflections | (Δ/σ)max < 0.001 |
205 parameters | Δρmax = 1.05 e Å−3 |
3 restraints | Δρmin = −0.58 e Å−3 |
Special details top
Experimental. CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
O8 | 0.48117 (12) | −0.10115 (11) | 0.50331 (15) | 0.0171 (3) | |
C9 | 0.13466 (16) | −0.15904 (15) | 0.3975 (2) | 0.0136 (4) | |
C3 | 0.35158 (17) | −0.03829 (15) | 0.2989 (2) | 0.0138 (4) | |
C2 | 0.15060 (18) | 0.18038 (16) | 0.2854 (2) | 0.0161 (5) | |
C1 | 0.05519 (17) | 0.12413 (16) | 0.1862 (2) | 0.0157 (5) | |
C5 | 0.17175 (17) | −0.19486 (16) | 0.2562 (2) | 0.0159 (4) | |
H5 | 0.1918 | −0.1763 | 0.2046 | 0.019* | |
C10 | 0.12408 (18) | −0.08675 (16) | 0.4695 (2) | 0.0164 (5) | |
H10A | 0.0509 | −0.0783 | 0.4332 | 0.02* | |
H10B | 0.1594 | −0.1061 | 0.5577 | 0.02* | |
C8 | 0.11430 (17) | −0.24836 (16) | 0.4050 (2) | 0.0166 (5) | |
H8 | 0.095 | −0.2658 | 0.4578 | 0.02* | |
C7 | 0.12253 (18) | −0.31226 (16) | 0.3342 (2) | 0.0191 (5) | |
H7 | 0.1085 | −0.3739 | 0.3375 | 0.023* | |
C4 | 0.40096 (16) | −0.05966 (15) | 0.4397 (2) | 0.0131 (4) | |
C6 | 0.15143 (18) | −0.28453 (16) | 0.2589 (2) | 0.0188 (5) | |
H6 | 0.1572 | −0.327 | 0.2094 | 0.023* | |
K1 | 0.58006 (4) | −0.15237 (4) | 0.40836 (5) | 0.01943 (14) | |
Cr1 | 0.20602 (3) | 0.00055 (2) | 0.34171 (3) | 0.01121 (11) | |
O7 | 0.34714 (12) | −0.03049 (11) | 0.47715 (14) | 0.0141 (3) | |
O1 | 0.06949 (12) | 0.03859 (11) | 0.19965 (15) | 0.0152 (3) | |
O5 | 0.25793 (12) | −0.01071 (11) | 0.23925 (15) | 0.0149 (3) | |
O3 | 0.23003 (12) | 0.13133 (11) | 0.36386 (15) | 0.0159 (3) | |
O6 | 0.39886 (13) | −0.04729 (11) | 0.25436 (15) | 0.0182 (4) | |
O4 | 0.14698 (14) | 0.26204 (11) | 0.28554 (18) | 0.0234 (4) | |
N1 | 0.16395 (14) | −0.13233 (13) | 0.32521 (18) | 0.0132 (4) | |
O2 | −0.02507 (13) | 0.16134 (12) | 0.10562 (16) | 0.0206 (4) | |
N2 | 0.16758 (15) | −0.00044 (13) | 0.46620 (18) | 0.0141 (4) | |
H2A | 0.2279 (15) | 0.0120 (18) | 0.5462 (18) | 0.017* | |
H2B | 0.1230 (17) | 0.0471 (15) | 0.447 (2) | 0.017* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
O8 | 0.0154 (8) | 0.0171 (8) | 0.0184 (8) | 0.0014 (6) | 0.0096 (7) | 0.0023 (7) |
C9 | 0.0095 (10) | 0.0164 (11) | 0.0119 (10) | 0.0012 (8) | 0.0045 (9) | 0.0015 (8) |
C3 | 0.0169 (11) | 0.0086 (10) | 0.0151 (11) | −0.0025 (8) | 0.0088 (9) | −0.0012 (8) |
C2 | 0.0175 (11) | 0.0165 (11) | 0.0200 (11) | 0.0000 (9) | 0.0142 (10) | 0.0020 (9) |
C1 | 0.0178 (11) | 0.0173 (11) | 0.0165 (11) | 0.0017 (9) | 0.0126 (10) | 0.0033 (9) |
C5 | 0.0143 (10) | 0.0194 (12) | 0.0146 (11) | −0.0003 (9) | 0.0089 (9) | −0.0034 (9) |
C10 | 0.0175 (11) | 0.0181 (11) | 0.0173 (11) | 0.0007 (9) | 0.0122 (10) | 0.0006 (9) |
C8 | 0.0144 (10) | 0.0190 (12) | 0.0152 (11) | −0.0013 (9) | 0.0079 (9) | 0.0033 (9) |
C7 | 0.0155 (11) | 0.0146 (11) | 0.0185 (11) | −0.0023 (9) | 0.0051 (9) | 0.0014 (9) |
C4 | 0.0138 (10) | 0.0123 (10) | 0.0144 (10) | −0.0028 (8) | 0.0090 (9) | 0.0001 (8) |
C6 | 0.0170 (11) | 0.0163 (11) | 0.0198 (12) | −0.0001 (9) | 0.0090 (10) | −0.0030 (9) |
K1 | 0.0199 (3) | 0.0196 (3) | 0.0208 (3) | 0.0009 (2) | 0.0130 (2) | −0.0016 (2) |
Cr1 | 0.01163 (18) | 0.01059 (18) | 0.01135 (18) | 0.00029 (13) | 0.00669 (15) | 0.00077 (13) |
O7 | 0.0129 (7) | 0.0172 (8) | 0.0124 (8) | 0.0013 (6) | 0.0074 (6) | 0.0008 (6) |
O1 | 0.0132 (7) | 0.0146 (8) | 0.0155 (8) | 0.0006 (6) | 0.0071 (7) | 0.0013 (6) |
O5 | 0.0159 (8) | 0.0168 (8) | 0.0126 (7) | 0.0011 (6) | 0.0086 (7) | 0.0018 (6) |
O3 | 0.0158 (8) | 0.0128 (8) | 0.0185 (8) | −0.0015 (6) | 0.0097 (7) | −0.0013 (6) |
O6 | 0.0232 (8) | 0.0181 (9) | 0.0185 (8) | −0.0021 (7) | 0.0151 (7) | −0.0013 (7) |
O4 | 0.0286 (9) | 0.0126 (8) | 0.0340 (10) | 0.0008 (7) | 0.0212 (9) | 0.0006 (7) |
N1 | 0.0126 (9) | 0.0122 (9) | 0.0134 (9) | 0.0009 (7) | 0.0067 (8) | 0.0009 (7) |
O2 | 0.0173 (8) | 0.0197 (9) | 0.0228 (9) | 0.0057 (7) | 0.0106 (7) | 0.0077 (7) |
N2 | 0.0165 (9) | 0.0126 (9) | 0.0135 (9) | 0.0018 (7) | 0.0089 (8) | 0.0001 (7) |
Geometric parameters (Å, º) top
O8—C4 | 1.220 (3) | C4—K1 | 3.440 (2) |
O8—K1 | 2.6514 (17) | C6—H6 | 0.95 |
C9—N1 | 1.347 (3) | K1—O4ii | 2.7287 (18) |
C9—C8 | 1.385 (3) | K1—O3iii | 2.7783 (17) |
C9—C10 | 1.507 (3) | K1—O6iv | 2.8276 (17) |
C3—O6 | 1.212 (3) | K1—O6 | 2.8567 (18) |
C3—O5 | 1.296 (3) | K1—O2v | 2.8803 (18) |
C3—C4 | 1.562 (3) | K1—O7iii | 2.9938 (17) |
C3—K1 | 3.512 (2) | K1—O4v | 3.2576 (19) |
C2—O4 | 1.215 (3) | K1—K1iv | 3.3815 (11) |
C2—O3 | 1.301 (3) | K1—C2ii | 3.501 (2) |
C2—C1 | 1.556 (3) | Cr1—O7 | 1.9557 (16) |
C2—K1i | 3.501 (2) | Cr1—O1 | 1.9614 (16) |
C1—O2 | 1.225 (3) | Cr1—O5 | 1.9681 (16) |
C1—O1 | 1.286 (3) | Cr1—O3 | 1.9700 (16) |
C5—N1 | 1.355 (3) | Cr1—N1 | 2.0581 (19) |
C5—C6 | 1.378 (3) | Cr1—N2 | 2.0644 (19) |
C5—H5 | 0.95 | Cr1—K1iii | 3.8121 (6) |
C10—N2 | 1.475 (3) | O7—K1iii | 2.9938 (17) |
C10—H10A | 0.99 | O3—K1iii | 2.7783 (17) |
C10—H10B | 0.99 | O6—K1iv | 2.8276 (17) |
C8—C7 | 1.390 (3) | O4—K1i | 2.7287 (18) |
C8—H8 | 0.95 | O4—K1vi | 3.2576 (19) |
C7—C6 | 1.382 (3) | O2—K1vi | 2.8803 (18) |
C7—H7 | 0.95 | N2—H2A | 0.944 (17) |
C4—O7 | 1.299 (3) | N2—H2B | 0.934 (17) |
| | | |
C4—O8—K1 | 120.82 (14) | O7iii—K1—K1iv | 114.31 (3) |
N1—C9—C8 | 121.9 (2) | O4v—K1—K1iv | 48.49 (3) |
N1—C9—C10 | 116.8 (2) | O8—K1—C4 | 17.73 (5) |
C8—C9—C10 | 121.3 (2) | O4ii—K1—C4 | 155.56 (6) |
O6—C3—O5 | 125.7 (2) | O3iii—K1—C4 | 107.44 (5) |
O6—C3—C4 | 121.5 (2) | O6iv—K1—C4 | 110.64 (5) |
O5—C3—C4 | 112.72 (18) | O6—K1—C4 | 44.14 (5) |
O6—C3—K1 | 48.47 (12) | O2v—K1—C4 | 98.23 (5) |
O5—C3—K1 | 166.81 (15) | O7iii—K1—C4 | 71.69 (5) |
C4—C3—K1 | 74.44 (11) | O4v—K1—C4 | 67.09 (5) |
O4—C2—O3 | 125.8 (2) | K1iv—K1—C4 | 93.35 (4) |
O4—C2—C1 | 120.9 (2) | O8—K1—C2ii | 150.54 (6) |
O3—C2—C1 | 113.4 (2) | O4ii—K1—C2ii | 17.46 (5) |
O4—C2—K1i | 42.36 (12) | O3iii—K1—C2ii | 97.26 (5) |
O3—C2—K1i | 117.88 (14) | O6iv—K1—C2ii | 79.97 (5) |
C1—C2—K1i | 109.81 (13) | O6—K1—C2ii | 122.39 (5) |
O2—C1—O1 | 125.4 (2) | O2v—K1—C2ii | 57.29 (5) |
O2—C1—C2 | 120.6 (2) | O7iii—K1—C2ii | 137.65 (5) |
O1—C1—C2 | 113.97 (19) | O4v—K1—C2ii | 83.24 (5) |
N1—C5—C6 | 122.0 (2) | K1iv—K1—C2ii | 69.58 (4) |
N1—C5—H5 | 119 | C4—K1—C2ii | 149.77 (5) |
C6—C5—H5 | 119 | O8—K1—C3 | 43.67 (5) |
N2—C10—C9 | 111.72 (18) | O4ii—K1—C3 | 131.87 (6) |
N2—C10—H10A | 109.3 | O3iii—K1—C3 | 128.22 (5) |
C9—C10—H10A | 109.3 | O6iv—K1—C3 | 89.22 (5) |
N2—C10—H10B | 109.3 | O6—K1—C3 | 18.52 (5) |
C9—C10—H10B | 109.3 | O2v—K1—C3 | 103.14 (5) |
H10A—C10—H10B | 107.9 | O7iii—K1—C3 | 77.10 (5) |
C9—C8—C7 | 119.2 (2) | O4v—K1—C3 | 55.76 (5) |
C9—C8—H8 | 120.4 | K1iv—K1—C3 | 68.49 (4) |
C7—C8—H8 | 120.4 | C4—K1—C3 | 25.94 (5) |
C6—C7—C8 | 118.8 (2) | C2ii—K1—C3 | 134.53 (6) |
C6—C7—H7 | 120.6 | O7—Cr1—O1 | 174.81 (7) |
C8—C7—H7 | 120.6 | O7—Cr1—O5 | 82.41 (7) |
O8—C4—O7 | 125.9 (2) | O1—Cr1—O5 | 93.64 (7) |
O8—C4—C3 | 121.04 (19) | O7—Cr1—O3 | 94.28 (7) |
O7—C4—C3 | 113.09 (18) | O1—Cr1—O3 | 82.56 (7) |
O8—C4—K1 | 41.45 (11) | O5—Cr1—O3 | 93.40 (7) |
O7—C4—K1 | 167.29 (15) | O7—Cr1—N1 | 90.36 (7) |
C3—C4—K1 | 79.62 (12) | O1—Cr1—N1 | 93.37 (7) |
C5—C6—C7 | 119.5 (2) | O5—Cr1—N1 | 95.33 (7) |
C5—C6—H6 | 120.3 | O3—Cr1—N1 | 170.59 (7) |
C7—C6—H6 | 120.3 | O7—Cr1—N2 | 90.37 (7) |
O8—K1—O4ii | 165.93 (6) | O1—Cr1—N2 | 93.78 (7) |
O8—K1—O3iii | 92.75 (5) | O5—Cr1—N2 | 171.88 (7) |
O4ii—K1—O3iii | 97.00 (5) | O3—Cr1—N2 | 90.81 (7) |
O8—K1—O6iv | 124.85 (5) | N1—Cr1—N2 | 80.95 (8) |
O4ii—K1—O6iv | 62.84 (5) | O7—Cr1—K1iii | 50.95 (5) |
O3iii—K1—O6iv | 102.04 (5) | O1—Cr1—K1iii | 126.61 (5) |
O8—K1—O6 | 61.83 (5) | O5—Cr1—K1iii | 96.15 (5) |
O4ii—K1—O6 | 115.54 (5) | O3—Cr1—K1iii | 44.60 (5) |
O3iii—K1—O6 | 136.76 (5) | N1—Cr1—K1iii | 137.33 (5) |
O6iv—K1—O6 | 71.85 (6) | N2—Cr1—K1iii | 82.02 (6) |
O8—K1—O2v | 93.31 (5) | C4—O7—Cr1 | 114.47 (14) |
O4ii—K1—O2v | 74.24 (5) | C4—O7—K1iii | 109.95 (13) |
O3iii—K1—O2v | 106.33 (5) | Cr1—O7—K1iii | 98.57 (6) |
O6iv—K1—O2v | 130.68 (5) | C1—O1—Cr1 | 115.29 (14) |
O6—K1—O2v | 109.32 (5) | C3—O5—Cr1 | 115.22 (14) |
O8—K1—O7iii | 70.70 (5) | C2—O3—Cr1 | 114.74 (15) |
O4ii—K1—O7iii | 123.12 (5) | C2—O3—K1iii | 138.21 (15) |
O3iii—K1—O7iii | 59.67 (5) | Cr1—O3—K1iii | 105.54 (7) |
O6iv—K1—O7iii | 72.18 (5) | C3—O6—K1iv | 144.76 (15) |
O6—K1—O7iii | 78.34 (5) | C3—O6—K1 | 113.01 (14) |
O2v—K1—O7iii | 156.95 (5) | K1iv—O6—K1 | 73.01 (4) |
O8—K1—O4v | 76.65 (5) | C2—O4—K1i | 120.18 (15) |
O4ii—K1—O4v | 90.49 (6) | C2—O4—K1vi | 114.95 (16) |
O3iii—K1—O4v | 156.02 (5) | K1i—O4—K1vi | 68.13 (4) |
O6iv—K1—O4v | 101.65 (5) | C9—N1—C5 | 118.7 (2) |
O6—K1—O4v | 56.12 (5) | C9—N1—Cr1 | 116.04 (15) |
O2v—K1—O4v | 53.93 (5) | C5—N1—Cr1 | 125.04 (16) |
O7iii—K1—O4v | 132.74 (4) | C1—O2—K1vi | 128.28 (16) |
O8—K1—K1iv | 110.14 (4) | C10—N2—Cr1 | 113.54 (14) |
O4ii—K1—K1iv | 63.38 (4) | C10—N2—H2A | 109.7 (17) |
O3iii—K1—K1iv | 153.36 (4) | Cr1—N2—H2A | 106.8 (17) |
O6iv—K1—K1iv | 53.89 (4) | C10—N2—H2B | 111.1 (17) |
O6—K1—K1iv | 53.10 (3) | Cr1—N2—H2B | 109.2 (17) |
O2v—K1—K1iv | 86.37 (4) | H2A—N2—H2B | 106 (2) |
| | | |
O4—C2—C1—O2 | 0.8 (3) | O5—Cr1—O7—C4 | −12.27 (15) |
O3—C2—C1—O2 | −179.5 (2) | O3—Cr1—O7—C4 | −105.14 (15) |
K1i—C2—C1—O2 | 46.4 (2) | N1—Cr1—O7—C4 | 83.06 (15) |
O4—C2—C1—O1 | −178.2 (2) | N2—Cr1—O7—C4 | 164.01 (15) |
O3—C2—C1—O1 | 1.6 (3) | K1iii—Cr1—O7—C4 | −116.59 (16) |
K1i—C2—C1—O1 | −132.58 (16) | O1—Cr1—O7—K1iii | 63.7 (8) |
N1—C9—C10—N2 | −11.1 (3) | O5—Cr1—O7—K1iii | 104.32 (6) |
C8—C9—C10—N2 | 169.4 (2) | O3—Cr1—O7—K1iii | 11.45 (6) |
N1—C9—C8—C7 | −1.1 (3) | N1—Cr1—O7—K1iii | −160.35 (6) |
C10—C9—C8—C7 | 178.3 (2) | N2—Cr1—O7—K1iii | −79.39 (7) |
C9—C8—C7—C6 | 0.4 (3) | O2—C1—O1—Cr1 | −178.10 (18) |
K1—O8—C4—O7 | −179.09 (16) | C2—C1—O1—Cr1 | 0.8 (2) |
K1—O8—C4—C3 | 2.3 (3) | O7—Cr1—O1—C1 | −54.6 (8) |
O6—C3—C4—O8 | −13.5 (3) | O5—Cr1—O1—C1 | −94.89 (15) |
O5—C3—C4—O8 | 166.7 (2) | O3—Cr1—O1—C1 | −1.93 (15) |
K1—C3—C4—O8 | −1.53 (18) | N1—Cr1—O1—C1 | 169.54 (15) |
O6—C3—C4—O7 | 167.7 (2) | N2—Cr1—O1—C1 | 88.40 (16) |
O5—C3—C4—O7 | −12.1 (3) | K1iii—Cr1—O1—C1 | 5.54 (17) |
K1—C3—C4—O7 | 179.67 (18) | O6—C3—O5—Cr1 | −177.78 (18) |
O6—C3—C4—K1 | −11.94 (19) | C4—C3—O5—Cr1 | 2.0 (2) |
O5—C3—C4—K1 | 168.26 (17) | K1—C3—O5—Cr1 | 122.8 (6) |
N1—C5—C6—C7 | −0.2 (4) | O7—Cr1—O5—C3 | 4.95 (15) |
C8—C7—C6—C5 | 0.3 (3) | O1—Cr1—O5—C3 | −178.43 (15) |
C4—O8—K1—O4ii | −79.5 (3) | O3—Cr1—O5—C3 | 98.81 (15) |
C4—O8—K1—O3iii | 146.59 (17) | N1—Cr1—O5—C3 | −84.70 (16) |
C4—O8—K1—O6iv | 39.85 (19) | N2—Cr1—O5—C3 | −22.4 (6) |
C4—O8—K1—O6 | 3.31 (16) | K1iii—Cr1—O5—C3 | 54.13 (15) |
C4—O8—K1—O2v | −106.86 (17) | O4—C2—O3—Cr1 | 176.61 (19) |
C4—O8—K1—O7iii | 90.13 (17) | C1—C2—O3—Cr1 | −3.2 (2) |
C4—O8—K1—O4v | −55.17 (17) | K1i—C2—O3—Cr1 | 127.09 (11) |
C4—O8—K1—K1iv | −19.52 (18) | O4—C2—O3—K1iii | 13.3 (4) |
C4—O8—K1—C2ii | −103.40 (19) | C1—C2—O3—K1iii | −166.50 (14) |
C4—O8—K1—C3 | −1.25 (15) | K1i—C2—O3—K1iii | −36.3 (2) |
O7—C4—K1—O8 | 3.4 (6) | O7—Cr1—O3—C2 | 178.75 (15) |
C3—C4—K1—O8 | −178.0 (2) | O1—Cr1—O3—C2 | 2.88 (15) |
O8—C4—K1—O4ii | 144.69 (17) | O5—Cr1—O3—C2 | 96.12 (15) |
O7—C4—K1—O4ii | 148.1 (6) | N1—Cr1—O3—C2 | −62.0 (5) |
C3—C4—K1—O4ii | −33.33 (19) | N2—Cr1—O3—C2 | −90.82 (16) |
O8—C4—K1—O3iii | −35.20 (18) | K1iii—Cr1—O3—C2 | −168.57 (18) |
O7—C4—K1—O3iii | −31.8 (7) | O7—Cr1—O3—K1iii | −12.68 (7) |
C3—C4—K1—O3iii | 146.77 (11) | O1—Cr1—O3—K1iii | 171.45 (7) |
O8—C4—K1—O6iv | −145.81 (16) | O5—Cr1—O3—K1iii | −95.31 (7) |
O7—C4—K1—O6iv | −142.4 (7) | N1—Cr1—O3—K1iii | 106.6 (4) |
C3—C4—K1—O6iv | 36.17 (12) | N2—Cr1—O3—K1iii | 77.75 (7) |
O8—C4—K1—O6 | −175.8 (2) | O5—C3—O6—K1iv | −71.9 (4) |
O7—C4—K1—O6 | −172.4 (7) | C4—C3—O6—K1iv | 108.4 (3) |
C3—C4—K1—O6 | 6.17 (10) | K1—C3—O6—K1iv | 92.9 (3) |
O8—C4—K1—O2v | 74.87 (17) | O5—C3—O6—K1 | −164.79 (18) |
O7—C4—K1—O2v | 78.2 (7) | C4—C3—O6—K1 | 15.4 (2) |
C3—C4—K1—O2v | −103.15 (11) | O8—K1—O6—C3 | −9.96 (15) |
O8—C4—K1—O7iii | −83.79 (17) | O4ii—K1—O6—C3 | 154.53 (15) |
O7—C4—K1—O7iii | −80.4 (7) | O3iii—K1—O6—C3 | −70.63 (17) |
C3—C4—K1—O7iii | 98.19 (11) | O6iv—K1—O6—C3 | −159.01 (15) |
O8—C4—K1—O4v | 119.88 (18) | O2v—K1—O6—C3 | 73.25 (16) |
O7—C4—K1—O4v | 123.2 (7) | O7iii—K1—O6—C3 | −84.16 (15) |
C3—C4—K1—O4v | −58.14 (11) | O4v—K1—O6—C3 | 82.56 (15) |
O8—C4—K1—K1iv | 161.69 (17) | K1iv—K1—O6—C3 | 142.95 (17) |
O7—C4—K1—K1iv | 165.1 (7) | C4—K1—O6—C3 | −8.51 (14) |
C3—C4—K1—K1iv | −16.33 (11) | C2ii—K1—O6—C3 | 136.14 (15) |
O8—C4—K1—C2ii | 108.13 (18) | O8—K1—O6—K1iv | −152.91 (6) |
O7—C4—K1—C2ii | 111.5 (7) | O4ii—K1—O6—K1iv | 11.58 (6) |
C3—C4—K1—C2ii | −69.89 (16) | O3iii—K1—O6—K1iv | 146.43 (6) |
O8—C4—K1—C3 | 178.0 (2) | O6iv—K1—O6—K1iv | 58.04 (5) |
O7—C4—K1—C3 | −178.6 (7) | O2v—K1—O6—K1iv | −69.70 (5) |
O6—C3—K1—O8 | 167.24 (19) | O7iii—K1—O6—K1iv | 132.89 (4) |
O5—C3—K1—O8 | −123.8 (7) | O4v—K1—O6—K1iv | −60.39 (5) |
C4—C3—K1—O8 | 0.87 (10) | C4—K1—O6—K1iv | −151.46 (8) |
O6—C3—K1—O4ii | −31.40 (18) | C2ii—K1—O6—K1iv | −6.81 (7) |
O5—C3—K1—O4ii | 37.5 (7) | C3—K1—O6—K1iv | −142.95 (17) |
C4—C3—K1—O4ii | 162.22 (11) | O3—C2—O4—K1i | −93.7 (2) |
O6—C3—K1—O3iii | 124.66 (15) | C1—C2—O4—K1i | 86.0 (2) |
O5—C3—K1—O3iii | −166.4 (6) | O3—C2—O4—K1vi | −171.93 (17) |
C4—C3—K1—O3iii | −41.71 (13) | C1—C2—O4—K1vi | 7.8 (3) |
O6—C3—K1—O6iv | 19.90 (15) | K1i—C2—O4—K1vi | −78.18 (13) |
O5—C3—K1—O6iv | 88.8 (7) | C8—C9—N1—C5 | 1.2 (3) |
C4—C3—K1—O6iv | −146.47 (12) | C10—C9—N1—C5 | −178.25 (19) |
O5—C3—K1—O6 | 68.9 (6) | C8—C9—N1—Cr1 | −173.43 (17) |
C4—C3—K1—O6 | −166.4 (2) | C10—C9—N1—Cr1 | 7.1 (2) |
O6—C3—K1—O2v | −111.88 (15) | C6—C5—N1—C9 | −0.5 (3) |
O5—C3—K1—O2v | −42.9 (7) | C6—C5—N1—Cr1 | 173.60 (17) |
C4—C3—K1—O2v | 81.75 (12) | O7—Cr1—N1—C9 | 89.21 (16) |
O6—C3—K1—O7iii | 91.78 (15) | O1—Cr1—N1—C9 | −94.40 (16) |
O5—C3—K1—O7iii | 160.7 (7) | O5—Cr1—N1—C9 | 171.62 (15) |
C4—C3—K1—O7iii | −74.59 (11) | O3—Cr1—N1—C9 | −30.4 (5) |
O6—C3—K1—O4v | −84.79 (16) | N2—Cr1—N1—C9 | −1.11 (15) |
O5—C3—K1—O4v | −15.8 (6) | K1iii—Cr1—N1—C9 | 66.55 (18) |
C4—C3—K1—O4v | 108.84 (12) | O7—Cr1—N1—C5 | −85.05 (18) |
O6—C3—K1—K1iv | −31.19 (14) | O1—Cr1—N1—C5 | 91.34 (18) |
O5—C3—K1—K1iv | 37.7 (6) | O5—Cr1—N1—C5 | −2.64 (18) |
C4—C3—K1—K1iv | 162.44 (12) | O3—Cr1—N1—C5 | 155.4 (4) |
O6—C3—K1—C4 | 166.4 (2) | N2—Cr1—N1—C5 | −175.37 (19) |
O5—C3—K1—C4 | −124.7 (7) | K1iii—Cr1—N1—C5 | −107.71 (17) |
O6—C3—K1—C2ii | −55.17 (18) | O1—C1—O2—K1vi | 167.30 (15) |
O5—C3—K1—C2ii | 13.8 (7) | C2—C1—O2—K1vi | −11.5 (3) |
C4—C3—K1—C2ii | 138.46 (11) | C9—C10—N2—Cr1 | 9.8 (2) |
O8—C4—O7—Cr1 | −162.60 (19) | O7—Cr1—N2—C10 | −95.39 (16) |
C3—C4—O7—Cr1 | 16.1 (2) | O1—Cr1—N2—C10 | 87.73 (16) |
K1—C4—O7—Cr1 | −165.3 (6) | O5—Cr1—N2—C10 | −68.3 (6) |
O8—C4—O7—K1iii | 87.6 (2) | O3—Cr1—N2—C10 | 170.33 (16) |
C3—C4—O7—K1iii | −93.70 (17) | N1—Cr1—N2—C10 | −5.09 (15) |
K1—C4—O7—K1iii | 84.8 (7) | K1iii—Cr1—N2—C10 | −145.81 (15) |
O1—Cr1—O7—C4 | −52.9 (8) | | |
Symmetry codes: (i) x−1/2, y+1/2, z; (ii) x+1/2, y−1/2, z; (iii) −x+1, −y, −z+1; (iv) −x+1, y, −z+1/2; (v) −x+1/2, y−1/2, −z+1/2; (vi) −x+1/2, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2A···O5vii | 0.94 (2) | 2.29 (2) | 2.988 (3) | 130 (2) |
N2—H2A···O6vii | 0.94 (2) | 2.56 (2) | 3.499 (3) | 175 (2) |
N2—H2B···O2viii | 0.93 (2) | 2.14 (2) | 3.070 (3) | 175 (2) |
N2—H2B···O1viii | 0.93 (2) | 2.52 (2) | 3.157 (3) | 125 (2) |
C8—H8···O8ix | 0.95 | 2.53 | 3.319 (3) | 140 |
C7—H7···O7ix | 0.95 | 2.54 | 3.232 (3) | 130 |
C6—H6···O3v | 0.95 | 2.59 | 3.386 (3) | 142 |
Symmetry codes: (v) −x+1/2, y−1/2, −z+1/2; (vii) x, −y, z+1/2; (viii) −x, y, −z+1/2; (ix) −x+1/2, −y−1/2, −z+1. |