Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805016843/lh6432sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805016843/lh6432Isup2.hkl |
CCDC reference: 277713
Key indicators
- Single-crystal X-ray study
- T = 303 K
- Mean (C-C) = 0.004 Å
- R factor = 0.034
- wR factor = 0.097
- Data-to-parameter ratio = 15.3
checkCIF/PLATON results
No syntax errors found
Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. turquoise CRYSC01_ALERT_1_C No recognised colour has been given for crystal colour. RADNW01_ALERT_1_C The radiation wavelength lies outside the expected range for the supplied radiation type. Expected range 0.71065-0.71075 Wavelength given = 0.71093 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT230_ALERT_2_C Hirshfeld Test Diff for N5 - C16 .. 5.15 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for V1 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.25 PLAT353_ALERT_3_C Long N-H Bond (0.87A) N3 - H3N ... 1.07 Ang. PLAT353_ALERT_3_C Long N-H Bond (0.87A) N6 - H6N ... 1.07 Ang. PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.838(10) ...... 3.00 su-Rat O2 -H2B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.838(10) ...... 3.00 su-Rat O2 -H2B 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.19(3), Rep 2.189(12) ...... 2.50 su-Rat H2A -CL3 1.555 2.566 PLAT736_ALERT_1_C H...A Calc 2.21(3), Rep 2.203(13) ...... 2.31 su-Rat H2B -CL4 1.555 2.566
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CAD-4 Diffractometer Control Software (Enraf–Nonius, 1993); cell refinement: CAD-4 Diffractometer Control Software; data reduction: CAD-4 Diffractometer Control Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON2003 (Spek, 1990, 2003) and ORTEP-3 (Farrugia, 1997, 2005); software used to prepare material for publication: SHELXL97.
(C10H10N3)2[VCl2O(H2O)2]Cl2 | Z = 2 |
Mr = 589.19 | F(000) = 602 |
Triclinic, P1 | Dx = 1.519 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71093 Å |
a = 7.838 (2) Å | Cell parameters from 25 reflections |
b = 9.609 (1) Å | θ = 3.2–10.1° |
c = 17.739 (3) Å | µ = 0.83 mm−1 |
α = 86.68 (1)° | T = 303 K |
β = 86.10 (2)° | Prism, turquoise |
γ = 75.32 (1)° | 0.25 × 0.15 × 0.10 mm |
V = 1288.3 (4) Å3 |
Enraf–Nonius CAD-4 diffractometer | 3771 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.024 |
Graphite monochromator | θmax = 26.0°, θmin = 1.2° |
ω/2θ scans | h = −9→3 |
Absorption correction: ψ scan (North et al., 1968) | k = −11→11 |
Tmin = 0.735, Tmax = 0.918 | l = −21→21 |
6971 measured reflections | 3 standard reflections every 120 min |
5048 independent reflections | intensity decay: 0.1% |
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) = 0.097 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.054P)2 + 0.4055P] where P = (Fo2 + 2Fc2)/3 |
5048 reflections | (Δ/σ)max = 0.001 |
331 parameters | Δρmax = 0.50 e Å−3 |
6 restraints | Δρmin = −0.39 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 | ||
C1 | 0.2356 (3) | 0.5770 (3) | −0.00722 (14) | 0.0451 (6) | |
C2 | 0.2178 (4) | 0.7260 (3) | −0.01530 (16) | 0.0554 (7) | |
H2 | 0.2441 | 0.7761 | 0.0239 | 0.067* | |
C3 | 0.1615 (4) | 0.7960 (3) | −0.08136 (17) | 0.0626 (8) | |
H3 | 0.1504 | 0.8946 | −0.0875 | 0.075* | |
C4 | 0.1202 (5) | 0.7218 (4) | −0.13987 (17) | 0.0633 (8) | |
H4 | 0.0805 | 0.7697 | −0.1849 | 0.076* | |
C5 | 0.1394 (4) | 0.5787 (3) | −0.12967 (16) | 0.0566 (7) | |
H5 | 0.1137 | 0.5275 | −0.1685 | 0.068* | |
C6 | 0.3150 (3) | 0.3568 (3) | 0.07531 (15) | 0.0470 (6) | |
C7 | 0.3717 (4) | 0.3015 (4) | 0.14605 (17) | 0.0596 (7) | |
H7 | 0.3932 | 0.3608 | 0.1820 | 0.072* | |
C8 | 0.3948 (5) | 0.1575 (4) | 0.1610 (2) | 0.0723 (9) | |
H8 | 0.4326 | 0.1169 | 0.2078 | 0.087* | |
C9 | 0.3622 (5) | 0.0725 (4) | 0.1070 (2) | 0.0806 (10) | |
H9 | 0.3779 | −0.0260 | 0.1164 | 0.097* | |
C10 | 0.3065 (5) | 0.1355 (4) | 0.0397 (2) | 0.0737 (9) | |
H10 | 0.2851 | 0.0772 | 0.0032 | 0.088* | |
C11 | 0.3392 (3) | 0.4737 (3) | 0.44131 (14) | 0.0393 (5) | |
C12 | 0.4408 (3) | 0.4686 (3) | 0.37369 (15) | 0.0481 (6) | |
H12 | 0.4528 | 0.5531 | 0.3481 | 0.058* | |
C13 | 0.5229 (4) | 0.3377 (3) | 0.34528 (15) | 0.0497 (6) | |
H13 | 0.5929 | 0.3332 | 0.3006 | 0.060* | |
C14 | 0.5027 (3) | 0.2115 (3) | 0.38255 (15) | 0.0480 (6) | |
H14 | 0.5576 | 0.1224 | 0.3631 | 0.058* | |
C15 | 0.4014 (3) | 0.2208 (3) | 0.44783 (14) | 0.0432 (6) | |
H15 | 0.3865 | 0.1369 | 0.4732 | 0.052* | |
C16 | 0.1544 (3) | 0.6259 (3) | 0.53953 (13) | 0.0400 (5) | |
C17 | 0.0865 (3) | 0.7673 (3) | 0.56181 (15) | 0.0450 (6) | |
H17 | 0.1088 | 0.8449 | 0.5325 | 0.054* | |
C18 | −0.0131 (4) | 0.7874 (3) | 0.62793 (16) | 0.0519 (7) | |
H18 | −0.0610 | 0.8801 | 0.6444 | 0.062* | |
C19 | −0.0432 (4) | 0.6706 (3) | 0.67057 (16) | 0.0532 (7) | |
H19 | −0.1095 | 0.6832 | 0.7163 | 0.064* | |
C20 | 0.0263 (4) | 0.5357 (3) | 0.64431 (15) | 0.0503 (6) | |
H20 | 0.0040 | 0.4571 | 0.6727 | 0.060* | |
N1 | 0.2911 (3) | 0.5019 (3) | 0.05707 (13) | 0.0534 (6) | |
H1N | 0.320 (4) | 0.551 (3) | 0.0920 (18) | 0.064* | |
N2 | 0.2807 (3) | 0.2758 (3) | 0.02265 (13) | 0.0567 (6) | |
N3 | 0.1948 (3) | 0.5081 (3) | −0.06445 (12) | 0.0473 (5) | |
H3N | 0.225 (4) | 0.398 (3) | −0.0447 (16) | 0.057* | |
N4 | 0.2567 (3) | 0.6006 (2) | 0.47345 (13) | 0.0475 (5) | |
H4N | 0.272 (4) | 0.675 (3) | 0.4466 (16) | 0.057* | |
N5 | 0.1246 (3) | 0.5121 (2) | 0.57994 (12) | 0.0461 (5) | |
N6 | 0.3214 (3) | 0.3497 (2) | 0.47687 (12) | 0.0400 (4) | |
H6N | 0.245 (4) | 0.380 (3) | 0.5282 (15) | 0.048* | |
O1 | 0.2079 (3) | −0.0399 (2) | 0.75522 (11) | 0.0624 (5) | |
O2 | −0.1269 (2) | 0.1593 (3) | 0.73546 (12) | 0.0730 (7) | |
H2A | −0.180 (4) | 0.150 (4) | 0.6974 (11) | 0.088* | |
H2B | −0.203 (3) | 0.203 (4) | 0.7670 (13) | 0.088* | |
O3 | 0.3382 (3) | 0.2104 (3) | 0.72630 (11) | 0.0621 (6) | |
H3A | 0.417 (3) | 0.189 (4) | 0.6911 (11) | 0.075* | |
H3B | 0.387 (3) | 0.233 (3) | 0.7626 (11) | 0.075* | |
V1 | 0.13210 (5) | 0.12565 (4) | 0.73736 (2) | 0.03288 (11) | |
Cl1 | 0.07551 (10) | 0.23032 (9) | 0.85385 (4) | 0.0619 (2) | |
Cl2 | 0.13293 (8) | 0.14329 (7) | 0.60732 (3) | 0.04341 (15) | |
Cl3 | 0.35957 (8) | 0.86934 (6) | 0.38838 (3) | 0.04221 (15) | |
Cl4 | 0.44189 (9) | 0.67355 (8) | 0.17119 (4) | 0.0577 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0397 (13) | 0.0554 (15) | 0.0407 (13) | −0.0146 (12) | 0.0055 (11) | −0.0041 (11) |
C2 | 0.0620 (18) | 0.0618 (17) | 0.0504 (15) | −0.0298 (14) | 0.0011 (13) | −0.0082 (13) |
C3 | 0.077 (2) | 0.0527 (17) | 0.0634 (18) | −0.0289 (16) | −0.0009 (16) | 0.0040 (14) |
C4 | 0.074 (2) | 0.071 (2) | 0.0503 (16) | −0.0281 (17) | −0.0094 (15) | 0.0096 (14) |
C5 | 0.0658 (19) | 0.0634 (18) | 0.0453 (15) | −0.0230 (15) | −0.0086 (13) | −0.0025 (13) |
C6 | 0.0405 (14) | 0.0523 (15) | 0.0475 (14) | −0.0108 (12) | −0.0006 (11) | −0.0025 (11) |
C7 | 0.0583 (18) | 0.068 (2) | 0.0537 (16) | −0.0151 (15) | −0.0144 (14) | −0.0028 (14) |
C8 | 0.070 (2) | 0.073 (2) | 0.066 (2) | −0.0035 (18) | −0.0172 (17) | 0.0112 (17) |
C9 | 0.091 (3) | 0.0523 (19) | 0.091 (3) | −0.0032 (18) | −0.016 (2) | 0.0055 (18) |
C10 | 0.092 (3) | 0.0536 (19) | 0.074 (2) | −0.0105 (17) | −0.0137 (19) | −0.0147 (16) |
C11 | 0.0346 (12) | 0.0390 (13) | 0.0458 (13) | −0.0085 (10) | −0.0112 (10) | −0.0075 (10) |
C12 | 0.0458 (14) | 0.0466 (15) | 0.0547 (15) | −0.0161 (12) | −0.0092 (12) | 0.0017 (12) |
C13 | 0.0410 (14) | 0.0620 (17) | 0.0464 (14) | −0.0127 (13) | −0.0006 (11) | −0.0081 (12) |
C14 | 0.0418 (14) | 0.0466 (15) | 0.0527 (15) | −0.0030 (11) | −0.0031 (12) | −0.0147 (12) |
C15 | 0.0444 (14) | 0.0359 (12) | 0.0484 (14) | −0.0058 (11) | −0.0088 (11) | −0.0068 (10) |
C16 | 0.0371 (12) | 0.0401 (13) | 0.0437 (13) | −0.0071 (10) | −0.0105 (10) | −0.0113 (10) |
C17 | 0.0444 (14) | 0.0332 (12) | 0.0580 (15) | −0.0066 (11) | −0.0123 (12) | −0.0094 (11) |
C18 | 0.0473 (15) | 0.0424 (14) | 0.0637 (17) | −0.0004 (12) | −0.0130 (13) | −0.0218 (12) |
C19 | 0.0474 (15) | 0.0596 (17) | 0.0497 (15) | −0.0044 (13) | −0.0051 (12) | −0.0162 (13) |
C20 | 0.0573 (17) | 0.0453 (15) | 0.0470 (14) | −0.0095 (13) | −0.0046 (12) | −0.0027 (11) |
N1 | 0.0642 (15) | 0.0598 (15) | 0.0426 (12) | −0.0232 (12) | −0.0099 (11) | −0.0133 (10) |
N2 | 0.0661 (15) | 0.0523 (14) | 0.0506 (13) | −0.0098 (12) | −0.0079 (11) | −0.0099 (10) |
N3 | 0.0506 (13) | 0.0516 (13) | 0.0412 (11) | −0.0141 (10) | −0.0019 (9) | −0.0085 (9) |
N4 | 0.0559 (14) | 0.0344 (11) | 0.0534 (13) | −0.0146 (10) | −0.0011 (11) | 0.0003 (9) |
N5 | 0.0522 (13) | 0.0360 (11) | 0.0493 (12) | −0.0089 (10) | −0.0048 (10) | −0.0042 (9) |
N6 | 0.0408 (11) | 0.0360 (10) | 0.0424 (11) | −0.0062 (9) | −0.0055 (9) | −0.0064 (8) |
O1 | 0.0846 (15) | 0.0427 (11) | 0.0543 (11) | −0.0075 (10) | −0.0024 (10) | 0.0043 (8) |
O2 | 0.0316 (10) | 0.137 (2) | 0.0537 (12) | −0.0191 (12) | 0.0028 (8) | −0.0461 (13) |
O3 | 0.0466 (11) | 0.1086 (17) | 0.0476 (11) | −0.0466 (12) | 0.0054 (9) | −0.0268 (11) |
V1 | 0.0316 (2) | 0.0362 (2) | 0.0333 (2) | −0.01211 (16) | −0.00178 (15) | −0.00509 (15) |
Cl1 | 0.0529 (4) | 0.0962 (6) | 0.0468 (4) | −0.0334 (4) | 0.0070 (3) | −0.0337 (4) |
Cl2 | 0.0460 (3) | 0.0529 (4) | 0.0358 (3) | −0.0202 (3) | −0.0044 (2) | −0.0016 (2) |
Cl3 | 0.0377 (3) | 0.0454 (3) | 0.0480 (3) | −0.0176 (3) | −0.0031 (2) | −0.0057 (2) |
Cl4 | 0.0396 (3) | 0.0751 (5) | 0.0636 (4) | −0.0173 (3) | −0.0019 (3) | −0.0354 (4) |
C1—N3 | 1.342 (3) | C14—C15 | 1.353 (4) |
C1—N1 | 1.350 (3) | C14—H14 | 0.9300 |
C1—C2 | 1.403 (4) | C15—N6 | 1.352 (3) |
C2—C3 | 1.360 (4) | C15—H15 | 0.9300 |
C2—H2 | 0.9300 | C16—N5 | 1.334 (3) |
C3—C4 | 1.393 (4) | C16—N4 | 1.372 (3) |
C3—H3 | 0.9300 | C16—C17 | 1.398 (3) |
C4—C5 | 1.348 (4) | C17—C18 | 1.359 (4) |
C4—H4 | 0.9300 | C17—H17 | 0.9300 |
C5—N3 | 1.347 (3) | C18—C19 | 1.378 (4) |
C5—H5 | 0.9300 | C18—H18 | 0.9300 |
C6—N2 | 1.332 (3) | C19—C20 | 1.368 (4) |
C6—N1 | 1.381 (4) | C19—H19 | 0.9300 |
C6—C7 | 1.391 (4) | C20—N5 | 1.331 (3) |
C7—C8 | 1.362 (5) | C20—H20 | 0.9300 |
C7—H7 | 0.9300 | N1—H1N | 0.87 (3) |
C8—C9 | 1.371 (5) | N3—H3N | 1.07 (3) |
C8—H8 | 0.9300 | N4—H4N | 0.86 (3) |
C9—C10 | 1.355 (5) | N6—H6N | 1.07 (3) |
C9—H9 | 0.9300 | O1—V1 | 1.5719 (19) |
C10—N2 | 1.332 (4) | O2—V1 | 1.9753 (19) |
C10—H10 | 0.9300 | O2—H2A | 0.837 (10) |
C11—N6 | 1.350 (3) | O2—H2B | 0.838 (10) |
C11—N4 | 1.364 (3) | O3—V1 | 1.9791 (18) |
C11—C12 | 1.390 (4) | O3—H3A | 0.845 (10) |
C12—C13 | 1.367 (4) | O3—H3B | 0.839 (10) |
C12—H12 | 0.9300 | V1—Cl2 | 2.3030 (8) |
C13—C14 | 1.386 (4) | V1—Cl1 | 2.3169 (8) |
C13—H13 | 0.9300 | ||
N3—C1—N1 | 119.4 (2) | N5—C16—N4 | 117.6 (2) |
N3—C1—C2 | 119.1 (2) | N5—C16—C17 | 122.9 (2) |
N1—C1—C2 | 121.5 (2) | N4—C16—C17 | 119.5 (2) |
C3—C2—C1 | 118.9 (3) | C18—C17—C16 | 117.6 (3) |
C3—C2—H2 | 120.6 | C18—C17—H17 | 121.2 |
C1—C2—H2 | 120.6 | C16—C17—H17 | 121.2 |
C2—C3—C4 | 120.8 (3) | C17—C18—C19 | 120.1 (2) |
C2—C3—H3 | 119.6 | C17—C18—H18 | 120.0 |
C4—C3—H3 | 119.6 | C19—C18—H18 | 120.0 |
C5—C4—C3 | 118.3 (3) | C20—C19—C18 | 118.7 (3) |
C5—C4—H4 | 120.8 | C20—C19—H19 | 120.6 |
C3—C4—H4 | 120.8 | C18—C19—H19 | 120.6 |
N3—C5—C4 | 121.5 (3) | N5—C20—C19 | 122.8 (3) |
N3—C5—H5 | 119.3 | N5—C20—H20 | 118.6 |
C4—C5—H5 | 119.3 | C19—C20—H20 | 118.6 |
N2—C6—N1 | 116.9 (2) | C1—N1—C6 | 129.6 (2) |
N2—C6—C7 | 122.9 (3) | C1—N1—H1N | 116 (2) |
N1—C6—C7 | 120.1 (3) | C6—N1—H1N | 114 (2) |
C8—C7—C6 | 117.9 (3) | C10—N2—C6 | 117.0 (3) |
C8—C7—H7 | 121.1 | C1—N3—C5 | 121.4 (2) |
C6—C7—H7 | 121.1 | C1—N3—H3N | 103.7 (15) |
C7—C8—C9 | 119.8 (3) | C5—N3—H3N | 134.8 (15) |
C7—C8—H8 | 120.1 | C11—N4—C16 | 130.0 (2) |
C9—C8—H8 | 120.1 | C11—N4—H4N | 113 (2) |
C10—C9—C8 | 118.5 (3) | C16—N4—H4N | 117 (2) |
C10—C9—H9 | 120.8 | C20—N5—C16 | 117.9 (2) |
C8—C9—H9 | 120.8 | C11—N6—C15 | 121.0 (2) |
N2—C10—C9 | 123.9 (3) | C11—N6—H6N | 105.8 (14) |
N2—C10—H10 | 118.1 | C15—N6—H6N | 133.1 (14) |
C9—C10—H10 | 118.1 | V1—O2—H2A | 124 (2) |
N6—C11—N4 | 118.5 (2) | V1—O2—H2B | 127 (2) |
N6—C11—C12 | 119.4 (2) | H2A—O2—H2B | 107.3 (16) |
N4—C11—C12 | 122.1 (2) | V1—O3—H3A | 123 (2) |
C13—C12—C11 | 119.2 (3) | V1—O3—H3B | 124 (2) |
C13—C12—H12 | 120.4 | H3A—O3—H3B | 106.1 (15) |
C11—C12—H12 | 120.4 | O1—V1—O2 | 106.87 (12) |
C12—C13—C14 | 120.6 (3) | O1—V1—O3 | 106.15 (12) |
C12—C13—H13 | 119.7 | O2—V1—O3 | 146.98 (12) |
C14—C13—H13 | 119.7 | O1—V1—Cl2 | 103.59 (8) |
C15—C14—C13 | 118.6 (2) | O2—V1—Cl2 | 86.12 (7) |
C15—C14—H14 | 120.7 | O3—V1—Cl2 | 86.13 (6) |
C13—C14—H14 | 120.7 | O1—V1—Cl1 | 105.55 (8) |
N6—C15—C14 | 121.3 (2) | O2—V1—Cl1 | 85.55 (6) |
N6—C15—H15 | 119.4 | O3—V1—Cl1 | 85.80 (6) |
C14—C15—H15 | 119.4 | Cl2—V1—Cl1 | 150.85 (3) |
N3—C1—C2—C3 | −0.8 (4) | N3—C1—N1—C6 | 0.2 (4) |
N1—C1—C2—C3 | 180.0 (3) | C2—C1—N1—C6 | 179.4 (3) |
C1—C2—C3—C4 | 0.7 (5) | N2—C6—N1—C1 | 0.6 (4) |
C2—C3—C4—C5 | −0.7 (5) | C7—C6—N1—C1 | −179.1 (3) |
C3—C4—C5—N3 | 0.8 (5) | C9—C10—N2—C6 | 1.1 (5) |
N2—C6—C7—C8 | 0.9 (5) | N1—C6—N2—C10 | 178.9 (3) |
N1—C6—C7—C8 | −179.4 (3) | C7—C6—N2—C10 | −1.4 (4) |
C6—C7—C8—C9 | 0.0 (5) | N1—C1—N3—C5 | −179.8 (3) |
C7—C8—C9—C10 | −0.3 (6) | C2—C1—N3—C5 | 0.9 (4) |
C8—C9—C10—N2 | −0.3 (6) | C4—C5—N3—C1 | −0.9 (4) |
N6—C11—C12—C13 | −1.0 (4) | N6—C11—N4—C16 | 0.7 (4) |
N4—C11—C12—C13 | 178.7 (2) | C12—C11—N4—C16 | −179.0 (3) |
C11—C12—C13—C14 | 1.2 (4) | N5—C16—N4—C11 | −1.4 (4) |
C12—C13—C14—C15 | −0.6 (4) | C17—C16—N4—C11 | 178.5 (2) |
C13—C14—C15—N6 | −0.3 (4) | C19—C20—N5—C16 | −0.6 (4) |
N5—C16—C17—C18 | 0.3 (4) | N4—C16—N5—C20 | 179.6 (2) |
N4—C16—C17—C18 | −179.5 (2) | C17—C16—N5—C20 | −0.2 (4) |
C16—C17—C18—C19 | 0.4 (4) | N4—C11—N6—C15 | −179.5 (2) |
C17—C18—C19—C20 | −1.1 (4) | C12—C11—N6—C15 | 0.2 (3) |
C18—C19—C20—N5 | 1.2 (4) | C14—C15—N6—C11 | 0.4 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1N···Cl4 | 0.87 (3) | 2.29 (3) | 3.149 (2) | 170 (3) |
N3—H3N···N2 | 1.07 (3) | 1.62 (3) | 2.608 (3) | 150 (2) |
N4—H4N···Cl3 | 0.86 (3) | 2.32 (3) | 3.168 (2) | 169 (3) |
N6—H6N···N5 | 1.07 (3) | 1.66 (3) | 2.624 (3) | 148 (2) |
O2—H2A···Cl3i | 0.84 (1) | 2.19 (1) | 3.016 (2) | 170 (3) |
O2—H2B···Cl4i | 0.84 (1) | 2.20 (1) | 3.026 (2) | 167 (3) |
O3—H3B···Cl4ii | 0.84 (1) | 2.22 (1) | 3.0259 (19) | 162 (3) |
O3—H3B···Cl4ii | 0.84 (1) | 2.22 (1) | 3.0259 (19) | 162 (3) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1. |
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