The crystal and molecular structure of the title compound, (CH
7N
4)(CH
8N
4)[SbCl
6], has been determined at 295 and 92 K. It is composed of isolated [SbCl
6]
3− octahedra and aminoguanidinium mono- and dications. One of four of the crystallographically inequivalent aminoguanidinium cations is disordered at both temperatures. Two crystallographically inequivalent [SbCl
6]
3− octahedra were found to possess three significantly longer Sb—Cl bonds than three other octahedra. The shorter bonds are in the range 2.456 (2)–2.577 (2) Å, whereas the longer ones are between 2.705 (2) and 2.931 (2) Å. Each short Sb—Cl bond is located
trans to a long bond. It is argued that this deformation is caused by N—H
Cl hydrogen bonds.
Supporting information
CCDC references: 163896; 163897
Data collection: Kuma Diffraction Software (KUMA, 1996) for Iat295K; Kuma Diffraction Software (Kuma, 1996) for Iat92K. For both compounds, cell refinement: Kuma Diffraction Software; data reduction: Kuma Diffraction Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.
(Iat295K) Aminoguanidinium(1+)(2+) heksachloroantimonate(III)
top
Crystal data top
(CH7N4)(CH8N4)[SbCl6] | F(000) = 944 |
Mr = 485.67 | Dx = 1.998 Mg m−3 Dm = 1.99 (1) Mg m−3 Dm measured by flotation method |
Monoclinic, Pc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.522 (2) Å | Cell parameters from 40 reflections |
b = 13.856 (3) Å | θ = 7–14° |
c = 15.544 (3) Å | µ = 2.70 mm−1 |
β = 94.75 (3)° | T = 295 K |
V = 1614.5 (6) Å3 | Irregular, colourless |
Z = 4 | 0.40 × 0.40 × 0.30 mm |
Data collection top
KM–4 Diffractometer | 5052 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 25.1°, θmin = 1.5° |
ω–θ scan | h = −8→8 |
Absorption correction: ψ scan (Sheldrick, 1990) | k = 0→16 |
Tmin = 0.446, Tmax = 0.368 | l = −18→18 |
5690 measured reflections | 2 standard reflections every 50 reflections |
5690 independent reflections | intensity decay: 1.0% |
Refinement top
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.024 | Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo2) + (0.030P)2 + 1.1741P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.065 | (Δ/σ)max = 0.002 |
S = 1.10 | Δρmax = 0.59 e Å−3 |
5690 reflections | Δρmin = −0.36 e Å−3 |
329 parameters | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
40 restraints | Extinction coefficient: 0.0045 (2) |
Primary atom site location: Patterson | Absolute structure: (Flack, 1983) |
Secondary atom site location: difference Fourier map | Absolute structure parameter: −0.04 (2) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sb1 | 0.22309 (4) | 0.24869 (2) | 0.49848 (2) | 0.03317 (13) | |
Cl1 | 0.1821 (3) | 0.08653 (10) | 0.43411 (11) | 0.0543 (4) | |
Cl2 | 0.3160 (2) | 0.43664 (9) | 0.57138 (9) | 0.0443 (3) | |
Cl3 | −0.0196 (2) | 0.32372 (12) | 0.39736 (10) | 0.0528 (4) | |
Cl4 | 0.5004 (2) | 0.18271 (11) | 0.61516 (11) | 0.0561 (4) | |
Cl5 | −0.0012 (2) | 0.21192 (12) | 0.61079 (11) | 0.0572 (4) | |
Cl6 | 0.4618 (2) | 0.29880 (10) | 0.38538 (10) | 0.0488 (3) | |
Sb2 | −0.22441 (3) | 0.73957 (2) | 0.50076 (2) | 0.03493 (12) | |
Cl7 | −0.4371 (2) | 0.69473 (12) | 0.60557 (10) | 0.0516 (4) | |
Cl8 | 0.0259 (2) | 0.79332 (12) | 0.37415 (11) | 0.0563 (4) | |
Cl9 | −0.1997 (3) | 0.90379 (11) | 0.56122 (11) | 0.0600 (4) | |
Cl10 | −0.3125 (3) | 0.55414 (10) | 0.42616 (11) | 0.0577 (4) | |
Cl11 | −0.4689 (2) | 0.79739 (11) | 0.39258 (10) | 0.0513 (4) | |
Cl12 | 0.0389 (2) | 0.65268 (10) | 0.61370 (9) | 0.0463 (3) | |
C1 | −0.2310 (8) | 0.4387 (4) | 0.6934 (4) | 0.0360 (12) | |
N1 | −0.3051 (7) | 0.3636 (3) | 0.7257 (3) | 0.0458 (11) | |
H11 | −0.3136 | 0.3615 | 0.7830 | 0.130 (8)* | |
H12 | −0.3489 | 0.3139 | 0.6931 | 0.130 (8)* | |
N2 | −0.1768 (7) | 0.5132 (4) | 0.7412 (3) | 0.0581 (13) | |
H21 | −0.1930 | 0.5140 | 0.7979 | 0.130 (8)* | |
H22 | −0.1225 | 0.5631 | 0.7171 | 0.130 (8)* | |
N3 | −0.2013 (8) | 0.4434 (3) | 0.6089 (3) | 0.0460 (12) | |
H3 | −0.1394 | 0.4927 | 0.5883 | 0.086 (13)* | |
N4 | −0.2817 (7) | 0.3757 (3) | 0.5513 (3) | 0.0438 (11) | |
H41 | −0.4016 | 0.3780 | 0.5480 | 0.092 (9)* | |
H42 | −0.2493 | 0.3140 | 0.5618 | 0.092 (9)* | |
H43 | −0.2481 | 0.3910 | 0.4988 | 0.092 (9)* | |
C2 | 0.2508 (8) | 0.5506 (4) | 0.3070 (4) | 0.0393 (13) | |
N5 | 0.2289 (7) | 0.6344 (3) | 0.2663 (3) | 0.0496 (13) | |
H51 | 0.2909 | 0.6433 | 0.2198 | 0.130 (8)* | |
H52 | 0.1915 | 0.6861 | 0.2949 | 0.130 (8)* | |
N6 | 0.2923 (7) | 0.4736 (3) | 0.2672 (3) | 0.0583 (14) | |
H61 | 0.2544 | 0.4767 | 0.2108 | 0.130 (8)* | |
H62 | 0.3089 | 0.4144 | 0.2903 | 0.130 (8)* | |
N7 | 0.2234 (8) | 0.5448 (3) | 0.3917 (3) | 0.0508 (14) | |
H7 | 0.2379 | 0.4882 | 0.4198 | 0.086 (13)* | |
N8 | 0.2633 (7) | 0.6232 (4) | 0.4478 (3) | 0.0461 (12) | |
H81 | 0.3802 | 0.6373 | 0.4483 | 0.092 (9)* | |
H82 | 0.2371 | 0.6072 | 0.5014 | 0.092 (9)* | |
H83 | 0.1984 | 0.6749 | 0.4295 | 0.092 (9)* | |
C3 | 0.2761 (10) | 0.0548 (5) | 0.1938 (5) | 0.0557 (17) | |
N9 | 0.2177 (9) | 0.1381 (4) | 0.2192 (4) | 0.0682 (17) | |
H91 | 0.2337 | 0.1414 | 0.2771 | 0.130 (8)* | |
H92 | 0.2033 | 0.1968 | 0.1947 | 0.130 (8)* | |
N10 | 0.3041 (9) | −0.0206 (4) | 0.2491 (4) | 0.0809 (19) | |
H101 | 0.2849 | −0.0134 | 0.3051 | 0.130 (8)* | |
H102 | 0.3435 | −0.0774 | 0.2300 | 0.130 (8)* | |
N11 | 0.3025 (9) | 0.0415 (4) | 0.1129 (4) | 0.0647 (16) | |
H111 | 0.3232 | −0.0214 | 0.1037 | 0.086 (13)* | |
N12 | 0.2686 (9) | 0.1151 (4) | 0.0566 (4) | 0.0657 (16) | |
H121 | 0.1794 | 0.1016 | 0.0161 | 0.130 (8)* | |
H122 | 0.3592 | 0.1339 | 0.0261 | 0.130 (8)* | |
C41 | −0.2711 (18) | 1.0688 (10) | 0.3362 (9) | 0.042 (3) | 0.60 |
C42 | −0.241 (3) | 1.0438 (16) | 0.3047 (16) | 0.046 (5) | 0.40 |
N13 | −0.2870 (10) | 1.1308 (4) | 0.2751 (4) | 0.079 (2) | |
H131 | −0.3188 | 1.1922 | 0.2849 | 0.130 (8)* | |
H132 | −0.2653 | 1.1121 | 0.2215 | 0.130 (8)* | |
N14 | −0.3009 (10) | 1.0930 (5) | 0.4250 (5) | 0.092 (2) | |
H141 | −0.3381 | 1.1524 | 0.4384 | 0.130 (8)* | |
H142 | −0.2836 | 1.0478 | 0.4664 | 0.130 (8)* | |
N151 | −0.2162 (12) | 0.9813 (7) | 0.3195 (6) | 0.054 (2) | 0.60 |
H151 | −0.2031 | 0.9356 | 0.3607 | 0.086 (13)* | 0.60 |
N152 | −0.249 (2) | 1.0244 (10) | 0.3831 (9) | 0.055 (3) | 0.40 |
H152 | −0.2185 | 0.9664 | 0.4057 | 0.086 (13)* | 0.40 |
N16 | −0.1830 (9) | 0.9632 (4) | 0.2420 (4) | 0.0782 (18) | |
H161 | −0.1455 | 0.9042 | 0.2272 | 0.130 (8)* | |
H162 | −0.1971 | 1.0100 | 0.2019 | 0.130 (8)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sb1 | 0.0402 (3) | 0.03043 (16) | 0.0289 (2) | 0.00185 (11) | 0.0031 (2) | 0.00077 (13) |
Cl1 | 0.0807 (12) | 0.0373 (7) | 0.0448 (8) | −0.0031 (7) | 0.0047 (8) | −0.0048 (6) |
Cl2 | 0.0628 (10) | 0.0387 (6) | 0.0325 (7) | 0.0068 (6) | 0.0099 (6) | 0.0015 (5) |
Cl3 | 0.0484 (8) | 0.0642 (9) | 0.0448 (8) | 0.0068 (7) | −0.0017 (6) | 0.0127 (7) |
Cl4 | 0.0579 (10) | 0.0463 (8) | 0.0620 (9) | −0.0079 (7) | −0.0083 (7) | 0.0099 (7) |
Cl5 | 0.0634 (10) | 0.0610 (9) | 0.0499 (9) | 0.0056 (8) | 0.0210 (7) | 0.0108 (7) |
Cl6 | 0.0535 (9) | 0.0494 (8) | 0.0445 (8) | 0.0098 (6) | 0.0105 (6) | 0.0026 (6) |
Sb2 | 0.0385 (3) | 0.03486 (17) | 0.0315 (2) | 0.00055 (17) | 0.0032 (2) | 0.00171 (18) |
Cl7 | 0.0484 (8) | 0.0656 (9) | 0.0424 (8) | −0.0015 (7) | 0.0136 (6) | 0.0054 (7) |
Cl8 | 0.0582 (9) | 0.0658 (10) | 0.0460 (8) | 0.0140 (8) | 0.0118 (7) | 0.0062 (7) |
Cl9 | 0.0869 (13) | 0.0443 (8) | 0.0491 (9) | −0.0063 (8) | 0.0074 (8) | −0.0096 (6) |
Cl10 | 0.0952 (14) | 0.0413 (7) | 0.0380 (8) | 0.0051 (8) | 0.0149 (8) | 0.0042 (6) |
Cl11 | 0.0446 (8) | 0.0599 (8) | 0.0478 (8) | −0.0004 (7) | −0.0063 (6) | 0.0144 (7) |
Cl12 | 0.0431 (7) | 0.0548 (8) | 0.0407 (7) | −0.0007 (6) | 0.0025 (6) | 0.0088 (6) |
C1 | 0.039 (3) | 0.036 (3) | 0.032 (3) | −0.003 (2) | 0.000 (2) | 0.008 (2) |
N1 | 0.057 (3) | 0.052 (3) | 0.028 (2) | −0.010 (2) | 0.005 (2) | 0.0036 (19) |
N2 | 0.082 (4) | 0.055 (3) | 0.038 (3) | −0.023 (3) | 0.009 (3) | −0.005 (2) |
N3 | 0.061 (3) | 0.045 (3) | 0.033 (3) | −0.010 (2) | 0.012 (2) | 0.001 (2) |
N4 | 0.047 (3) | 0.053 (3) | 0.031 (3) | −0.002 (2) | 0.004 (2) | 0.008 (2) |
C2 | 0.043 (3) | 0.043 (3) | 0.031 (3) | −0.004 (2) | −0.001 (2) | 0.005 (2) |
N5 | 0.076 (4) | 0.045 (3) | 0.028 (2) | 0.006 (2) | 0.004 (2) | 0.0054 (19) |
N6 | 0.087 (4) | 0.043 (3) | 0.041 (3) | 0.009 (3) | −0.011 (3) | −0.002 (2) |
N7 | 0.076 (4) | 0.043 (3) | 0.032 (3) | −0.015 (2) | −0.004 (2) | 0.009 (2) |
N8 | 0.055 (3) | 0.056 (3) | 0.028 (3) | −0.008 (2) | 0.009 (2) | 0.000 (2) |
C3 | 0.054 (4) | 0.067 (4) | 0.045 (4) | −0.001 (3) | −0.001 (3) | −0.009 (3) |
N9 | 0.104 (5) | 0.050 (3) | 0.049 (3) | 0.019 (3) | 0.000 (3) | −0.010 (2) |
N10 | 0.119 (6) | 0.067 (4) | 0.059 (4) | 0.032 (4) | 0.018 (4) | 0.002 (3) |
N11 | 0.086 (4) | 0.051 (3) | 0.058 (4) | 0.004 (3) | 0.013 (3) | −0.006 (3) |
N12 | 0.088 (4) | 0.046 (3) | 0.064 (4) | −0.001 (3) | 0.010 (3) | 0.004 (3) |
C41 | 0.044 (7) | 0.040 (7) | 0.043 (8) | 0.008 (5) | 0.006 (5) | 0.010 (6) |
C42 | 0.041 (9) | 0.036 (11) | 0.061 (14) | 0.007 (8) | 0.011 (9) | −0.004 (9) |
N13 | 0.144 (7) | 0.049 (3) | 0.046 (3) | 0.026 (3) | 0.017 (4) | 0.013 (3) |
N14 | 0.122 (6) | 0.063 (4) | 0.098 (6) | 0.040 (4) | 0.051 (5) | 0.018 (4) |
N151 | 0.069 (6) | 0.043 (5) | 0.050 (5) | 0.009 (4) | 0.011 (4) | 0.010 (4) |
N152 | 0.087 (10) | 0.036 (6) | 0.041 (7) | −0.002 (6) | 0.000 (6) | 0.008 (6) |
N16 | 0.117 (5) | 0.057 (3) | 0.059 (4) | 0.005 (3) | −0.002 (4) | 0.005 (3) |
Geometric parameters (Å, º) top
Sb1—Cl1 | 2.469 (2) | N7—H7 | 0.9000 |
Sb1—Cl2 | 2.902 (2) | N8—H81 | 0.9000 |
Sb1—Cl3 | 2.532 (2) | N8—H82 | 0.9000 |
Sb1—Cl4 | 2.802 (2) | N8—H83 | 0.9000 |
Sb1—Cl5 | 2.577 (2) | C3—N9 | 1.308 (8) |
Sb1—Cl6 | 2.705 (2) | C3—N10 | 1.359 (9) |
Sb2—Cl7 | 2.456 (2) | C3—N11 | 1.302 (9) |
Sb2—Cl8 | 2.931 (2) | N11—N12 | 1.354 (8) |
Sb2—Cl9 | 2.463 (2) | N9—H91 | 0.9000 |
Sb2—Cl10 | 2.874 (2) | N9—H92 | 0.9001 |
Sb2—Cl11 | 2.518 (2) | N10—H101 | 0.9000 |
Sb2—Cl12 | 2.807 (2) | N10—H102 | 0.9000 |
C1—N1 | 1.301 (7) | N11—H111 | 0.9000 |
C1—N2 | 1.316 (7) | N12—H121 | 0.9000 |
C1—N3 | 1.352 (7) | N12—H122 | 0.9001 |
N3—N4 | 1.399 (7) | C41—N13 | 1.279 (15) |
N1—H11 | 0.9000 | C41—N14 | 1.455 (15) |
N1—H12 | 0.9000 | C41—N151 | 1.314 (15) |
N2—H21 | 0.9000 | C42—N152 | 1.25 (3) |
N2—H22 | 0.9000 | C42—N13 | 1.33 (2) |
N3—H3 | 0.9000 | C42—N16 | 1.57 (2) |
N4—H41 | 0.9000 | N13—H131 | 0.9000 |
N4—H42 | 0.9000 | N13—H132 | 0.9000 |
N4—H43 | 0.9000 | N14—N152 | 1.232 (15) |
C2—N5 | 1.327 (7) | N14—H141 | 0.9000 |
C2—N6 | 1.284 (7) | N14—H142 | 0.8999 |
C2—N7 | 1.352 (7) | N151—N16 | 1.275 (10) |
N7—N8 | 1.409 (7) | N151—H151 | 0.9000 |
N5—H51 | 0.9000 | N152—H152 | 0.9001 |
N5—H52 | 0.8999 | N16—H161 | 0.9000 |
N6—H61 | 0.9000 | N16—H162 | 0.9000 |
N6—H62 | 0.9001 | | |
| | | |
Cl1—Sb1—Cl2 | 173.19 (6) | N6—C2—N5 | 121.5 (5) |
Cl1—Sb1—Cl3 | 93.59 (6) | N6—C2—N7 | 118.9 (5) |
Cl1—Sb1—Cl4 | 91.53 (5) | N7—N8—H81 | 109.4 |
Cl1—Sb1—Cl5 | 91.59 (6) | N7—N8—H82 | 109.4 |
Cl1—Sb1—Cl6 | 92.15 (6) | N7—N8—H83 | 109.7 |
Cl2—Sb1—Cl3 | 90.68 (5) | N8—N7—H7 | 111.1 |
Cl2—Sb1—Cl4 | 84.13 (5) | H51—N5—H52 | 119.5 |
Cl2—Sb1—Cl5 | 93.61 (5) | H61—N6—H62 | 117.0 |
Cl2—Sb1—Cl6 | 82.65 (5) | H81—N8—H82 | 109.5 |
Cl3—Sb1—Cl4 | 174.79 (5) | H81—N8—H83 | 109.5 |
Cl3—Sb1—Cl5 | 91.31 (6) | H82—N8—H83 | 109.5 |
Cl3—Sb1—Cl6 | 88.54 (5) | C3—N9—H91 | 109.0 |
Cl4—Sb1—Cl5 | 89.49 (6) | C3—N9—H92 | 134.5 |
Cl4—Sb1—Cl6 | 90.33 (5) | C3—N10—H101 | 119.9 |
Cl5—Sb1—Cl6 | 176.25 (5) | C3—N10—H102 | 120.1 |
Cl7—Sb2—Cl8 | 179.34 (5) | C3—N11—N12 | 118.9 (6) |
Cl7—Sb2—Cl9 | 90.77 (6) | C3—N11—H111 | 109.4 |
Cl7—Sb2—Cl10 | 84.28 (5) | N9—C3—N10 | 121.7 (6) |
Cl7—Sb2—Cl11 | 92.51 (6) | N11—C3—N9 | 119.9 (7) |
Cl7—Sb2—Cl12 | 86.63 (5) | N11—C3—N10 | 118.3 (6) |
Cl8—Sb2—Cl9 | 89.37 (6) | N11—N12—H121 | 112.7 |
Cl8—Sb2—Cl10 | 95.50 (5) | N11—N12—H122 | 116.6 |
Cl8—Sb2—Cl11 | 86.85 (5) | N12—N11—H111 | 130.8 |
Cl8—Sb2—Cl12 | 93.99 (5) | H91—N9—H92 | 112.2 |
Cl9—Sb2—Cl10 | 170.96 (7) | H101—N10—H102 | 120.0 |
Cl9—Sb2—Cl11 | 89.36 (6) | H121—N12—H122 | 104.2 |
Cl9—Sb2—Cl12 | 97.50 (6) | C41—N13—H131 | 121.2 |
Cl10—Sb2—Cl11 | 83.32 (5) | C41—N13—H132 | 118.8 |
Cl10—Sb2—Cl12 | 89.77 (5) | C41—N14—H141 | 120.4 |
Cl11—Sb2—Cl12 | 173.10 (5) | C41—N14—H142 | 119.6 |
C1—N1—H11 | 118.4 | C41—N151—H151 | 121.8 |
C1—N1—H12 | 122.9 | C42—N13—H131 | 149.9 |
C1—N2—H21 | 120.1 | C42—N13—H132 | 89.9 |
C1—N2—H22 | 119.9 | C42—N152—H152 | 122.6 |
C1—N3—N4 | 119.5 (5) | C42—N16—H161 | 156.1 |
C1—N3—H3 | 120.9 | C42—N16—H162 | 83.9 |
N1—C1—N2 | 122.2 (5) | N13—C41—N151 | 119.0 (12) |
N1—C1—N3 | 121.5 (5) | N13—C41—N14 | 122.5 (10) |
N2—C1—N3 | 116.3 (5) | N13—C42—N16 | 120.6 (18) |
N3—N4—H41 | 113.1 | N14—N152—C42 | 113.1 (16) |
N3—N4—H42 | 115.2 | N14—N152—H142 | 39.8 |
N3—N4—H43 | 106.5 | N14—N152—H152 | 124.3 |
N4—N3—H3 | 119.3 | N151—C41—N14 | 118.4 (11) |
H11—N1—H12 | 118.7 | N151—N16—H161 | 120.6 |
H21—N2—H22 | 120.0 | N151—N16—H162 | 119.4 |
H41—N4—H42 | 107.4 | N152—C42—N13 | 120.0 (18) |
H41—N4—H43 | 107.1 | N152—C42—N16 | 119.4 (19) |
H42—N4—H43 | 107.2 | N152—N14—H141 | 161.0 |
C2—N5—H51 | 116.7 | N152—N14—H142 | 79.0 |
C2—N5—H52 | 119.5 | N16—N151—C41 | 117.2 (10) |
C2—N6—H61 | 111.1 | N16—N151—H151 | 121.0 |
C2—N6—H62 | 126.5 | H131—N13—H132 | 120.0 |
C2—N7—N8 | 121.0 (5) | H141—N14—H142 | 120.0 |
C2—N7—H7 | 120.1 | H142—N152—H152 | 84.5 |
N5—C2—N7 | 119.5 (5) | H161—N16—H162 | 120.0 |
| | | |
N1—C1—N3—N4 | 12.7 (9) | N10—C3—N11—N12 | 177.5 (7) |
N2—C1—N3—N4 | −169.0 (5) | N13—C41—N151—N16 | −0.5 (18) |
N6—C2—N7—N8 | 148.7 (6) | N14—C41—N151—N16 | −176.8 (9) |
N5—C2—N7—N8 | −33.4 (9) | N13—C42—N152—N14 | 0 (3) |
N9—C3—N11—N12 | 0.0 (11) | N16—C42—N152—N14 | −178.3 (14) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H12···Cl4i | 0.90 | 2.41 | 3.310 (5) | 173 |
N1—H11···Cl10ii | 0.90 | 2.51 | 3.323 (5) | 150 |
N2—H22···Cl12 | 0.90 | 2.43 | 3.291 (5) | 159 |
N2—H21···Cl10ii | 0.90 | 2.44 | 3.266 (5) | 152 |
N4—H41···Cl2i | 0.90 | 2.33 | 3.182 (5) | 158 |
N4—H42···Cl5 | 0.90 | 2.41 | 3.183 (5) | 144 |
N5—H52···Cl8 | 0.90 | 2.35 | 3.227 (5) | 164 |
N5—H51···Cl2iii | 0.90 | 2.58 | 3.303 (5) | 138 |
N6—H62···Cl6 | 0.90 | 2.41 | 3.238 (5) | 154 |
N7—H7···Cl2 | 0.90 | 2.49 | 3.195 (5) | 136 |
N8—H83···Cl8 | 0.90 | 2.22 | 3.118 (6) | 174 |
N8—H82···Cl12 | 0.90 | 2.47 | 3.223 (5) | 142 |
N8—H81···Cl10iv | 0.90 | 2.63 | 3.374 (6) | 141 |
N11—H111···Cl4v | 0.90 | 2.60 | 3.444 (6) | 157 |
Symmetry codes: (i) x−1, y, z; (ii) x, −y+1, z+1/2; (iii) x, −y+1, z−1/2; (iv) x+1, y, z; (v) x, −y, z−1/2. |
(Iat92K) Aminoguanidinium(1+)(2+) heksachloroantimonate(III)
top
Crystal data top
(CH7N4)(CH8N4)[SbCl6] | F(000) = 944 |
Mr = 485.67 | Dx = 2.047 Mg m−3 |
Monoclinic, Pc | Mo Kα radiation, λ = 0.71073 Å |
a = 7.426 (2) Å | Cell parameters from 40 reflections |
b = 13.836 (3) Å | θ = 7–14° |
c = 15.403 (3) Å | µ = 2.76 mm−1 |
β = 95.27 (3)° | T = 92 K |
V = 1575.9 (6) Å3 | Irregular, colourless |
Z = 4 | 0.40 × 0.40 × 0.30 mm |
Data collection top
KUMA KM–4 Diffractometer | 5334 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 25.1°, θmin = 1.5° |
ω–θ scan | h = −8→8 |
Absorption correction: ψ scan (Sheldrick, 1990) | k = −16→0 |
Tmin = 0.360, Tmax = 0.437 | l = −18→17 |
5579 measured reflections | 2 standard reflections every 50 reflections |
5579 independent reflections | intensity decay: 1.1% |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.019 | H-atom parameters constrained |
wR(F2) = 0.048 | Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo2) + (0.0216P)2 + 2.2178P] where P = (Fo2 + 2Fc2)/3 |
S = 1.09 | (Δ/σ)max = 0.001 |
5579 reflections | Δρmax = 0.48 e Å−3 |
319 parameters | Δρmin = −0.56 e Å−3 |
27 restraints | Absolute structure: (Flack, 1983) |
Primary atom site location: Patterson | Absolute structure parameter: −0.026 (15) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sb1 | 0.21663 (3) | 0.24731 (2) | 0.50009 (2) | 0.01226 (7) | |
Cl1 | 0.16847 (15) | 0.08646 (7) | 0.43343 (7) | 0.0197 (2) | |
Cl2 | 0.31288 (14) | 0.43630 (7) | 0.57333 (6) | 0.01589 (19) | |
Cl3 | −0.02444 (13) | 0.32359 (7) | 0.39779 (6) | 0.0187 (2) | |
Cl4 | 0.50038 (14) | 0.17844 (7) | 0.61877 (7) | 0.0210 (2) | |
Cl5 | −0.00845 (14) | 0.21124 (7) | 0.61105 (7) | 0.0219 (2) | |
Cl6 | 0.46172 (13) | 0.29562 (7) | 0.38473 (6) | 0.0180 (2) | |
Sb2 | −0.21786 (2) | 0.73996 (2) | 0.49897 (1) | 0.01230 (7) | |
Cl7 | −0.43114 (13) | 0.69876 (7) | 0.60558 (6) | 0.0179 (2) | |
Cl8 | 0.03592 (14) | 0.79826 (7) | 0.37311 (7) | 0.0203 (2) | |
Cl9 | −0.19014 (16) | 0.90405 (7) | 0.55862 (7) | 0.0221 (2) | |
Cl10 | −0.32523 (15) | 0.55302 (7) | 0.42652 (7) | 0.0192 (2) | |
Cl11 | −0.46382 (13) | 0.79786 (7) | 0.39081 (6) | 0.01658 (19) | |
Cl12 | 0.04560 (13) | 0.65015 (7) | 0.61760 (6) | 0.01566 (19) | |
C1 | −0.2339 (6) | 0.4386 (3) | 0.6944 (3) | 0.0145 (8) | |
N1 | −0.3151 (4) | 0.3646 (2) | 0.7274 (2) | 0.0156 (7) | |
H11 | −0.3198 | 0.3640 | 0.7856 | 0.051 (4)* | |
H12 | −0.3706 | 0.3151 | 0.6980 | 0.051 (4)* | |
N2 | −0.1783 (4) | 0.5131 (2) | 0.7429 (2) | 0.0194 (7) | |
H21 | −0.1816 | 0.5063 | 0.8008 | 0.051 (4)* | |
H22 | −0.1412 | 0.5673 | 0.7176 | 0.051 (4)* | |
N3 | −0.1992 (5) | 0.4407 (2) | 0.6096 (2) | 0.0170 (7) | |
H3 | −0.1778 | 0.4975 | 0.5838 | 0.021 (6)* | |
N4 | −0.2892 (5) | 0.3740 (3) | 0.5504 (2) | 0.0179 (8) | |
H41 | −0.4094 | 0.3800 | 0.5525 | 0.039 (6)* | |
H42 | −0.2520 | 0.3151 | 0.5692 | 0.039 (6)* | |
H43 | −0.3054 | 0.3802 | 0.4920 | 0.039 (6)* | |
C2 | 0.2442 (5) | 0.5527 (3) | 0.3096 (3) | 0.0158 (8) | |
N5 | 0.2253 (5) | 0.6343 (2) | 0.2676 (2) | 0.0164 (7) | |
H51 | 0.2572 | 0.6366 | 0.2127 | 0.051 (4)* | |
H52 | 0.1772 | 0.6867 | 0.2912 | 0.051 (4)* | |
N6 | 0.2853 (5) | 0.4718 (2) | 0.2716 (2) | 0.0193 (7) | |
H61 | 0.2552 | 0.4707 | 0.2136 | 0.051 (4)* | |
H62 | 0.3161 | 0.4168 | 0.3004 | 0.051 (4)* | |
N7 | 0.2093 (5) | 0.5466 (2) | 0.3952 (2) | 0.0172 (7) | |
H7 | 0.2510 | 0.4946 | 0.4258 | 0.021 (6)* | |
N8 | 0.2636 (5) | 0.6259 (2) | 0.4510 (2) | 0.0159 (7) | |
H81 | 0.3837 | 0.6262 | 0.4658 | 0.039 (6)* | |
H82 | 0.2290 | 0.6222 | 0.5053 | 0.039 (6)* | |
H83 | 0.2355 | 0.6845 | 0.4282 | 0.039 (6)* | |
C3 | 0.2785 (6) | 0.0559 (3) | 0.1963 (3) | 0.0193 (9) | |
N9 | 0.2154 (5) | 0.1391 (3) | 0.2207 (2) | 0.0209 (8) | |
H91 | 0.2056 | 0.1530 | 0.2771 | 0.051 (4)* | |
H92 | 0.2112 | 0.1856 | 0.1798 | 0.051 (4)* | |
N10 | 0.3108 (5) | −0.0167 (3) | 0.2520 (2) | 0.0246 (8) | |
H101 | 0.3022 | −0.0018 | 0.3083 | 0.051 (4)* | |
H102 | 0.3684 | −0.0678 | 0.2313 | 0.051 (4)* | |
N11 | 0.3114 (5) | 0.0419 (3) | 0.1131 (2) | 0.0174 (7) | |
H111 | 0.3397 | −0.0202 | 0.1033 | 0.021 (6)* | |
N12 | 0.2699 (5) | 0.1169 (2) | 0.0527 (2) | 0.0222 (8) | |
H121 | 0.1863 | 0.1040 | 0.0082 | 0.051 (4)* | |
H122 | 0.3629 | 0.1262 | 0.0201 | 0.051 (4)* | |
C4 | −0.2714 (7) | 1.0646 (4) | 0.3292 (4) | 0.0408 (15) | |
N13 | −0.2955 (5) | 1.1322 (2) | 0.2730 (2) | 0.0213 (8) | |
H131 | −0.3364 | 1.1903 | 0.2887 | 0.051 (4)* | |
H132 | −0.2711 | 1.1218 | 0.2176 | 0.051 (4)* | |
N14 | −0.3162 (6) | 1.0891 (3) | 0.4194 (3) | 0.0425 (13) | |
H141 | −0.3567 | 1.1486 | 0.4312 | 0.051 (4)* | |
H142 | −0.3026 | 1.0443 | 0.4619 | 0.051 (4)* | |
N151 | −0.2085 (6) | 0.9824 (3) | 0.3178 (3) | 0.0193 (9) | 0.75 |
H151 | −0.1932 | 0.9383 | 0.3608 | 0.021 (6)* | 0.75 |
N152 | −0.2463 (18) | 1.0219 (11) | 0.3857 (9) | 0.020 (3) | 0.25 |
H152 | −0.2500 | 1.0128 | 0.4434 | 0.021 (6)* | 0.25 |
N16 | −0.1662 (5) | 0.9643 (3) | 0.2374 (2) | 0.0317 (9) | |
H161 | −0.0499 | 0.9572 | 0.2266 | 0.051 (4)* | |
H162 | −0.2533 | 0.9548 | 0.1936 | 0.051 (4)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sb1 | 0.01483 (15) | 0.01068 (12) | 0.01142 (14) | 0.00152 (9) | 0.00200 (12) | 0.00028 (9) |
Cl1 | 0.0291 (6) | 0.0134 (4) | 0.0170 (5) | −0.0010 (4) | 0.0035 (4) | −0.0016 (4) |
Cl2 | 0.0215 (5) | 0.0151 (4) | 0.0115 (4) | 0.0021 (4) | 0.0041 (4) | 0.0010 (3) |
Cl3 | 0.0179 (5) | 0.0224 (5) | 0.0159 (5) | 0.0029 (4) | 0.0017 (4) | 0.0046 (4) |
Cl4 | 0.0217 (5) | 0.0158 (5) | 0.0250 (5) | −0.0028 (4) | −0.0005 (4) | 0.0042 (4) |
Cl5 | 0.0236 (5) | 0.0238 (5) | 0.0196 (5) | 0.0035 (4) | 0.0089 (4) | 0.0044 (4) |
Cl6 | 0.0205 (5) | 0.0167 (5) | 0.0175 (5) | 0.0039 (4) | 0.0059 (4) | 0.0005 (4) |
Sb2 | 0.01313 (14) | 0.01184 (12) | 0.01204 (14) | 0.00000 (11) | 0.00177 (12) | 0.00080 (11) |
Cl7 | 0.0156 (5) | 0.0238 (5) | 0.0148 (5) | −0.0017 (4) | 0.0040 (4) | 0.0013 (4) |
Cl8 | 0.0200 (5) | 0.0261 (5) | 0.0152 (5) | 0.0055 (4) | 0.0044 (4) | 0.0012 (4) |
Cl9 | 0.0282 (6) | 0.0201 (5) | 0.0182 (5) | −0.0038 (4) | 0.0034 (4) | −0.0042 (4) |
Cl10 | 0.0243 (5) | 0.0166 (5) | 0.0174 (5) | 0.0044 (4) | 0.0069 (4) | 0.0034 (4) |
Cl11 | 0.0140 (4) | 0.0189 (5) | 0.0166 (4) | −0.0002 (4) | 0.0002 (3) | 0.0030 (4) |
Cl12 | 0.0145 (5) | 0.0195 (5) | 0.0133 (4) | −0.0001 (4) | 0.0027 (3) | 0.0031 (4) |
C1 | 0.014 (2) | 0.0148 (19) | 0.0151 (19) | 0.0010 (16) | 0.0022 (15) | 0.0009 (16) |
N1 | 0.0156 (16) | 0.0178 (17) | 0.0138 (16) | −0.0024 (14) | 0.0032 (14) | 0.0016 (13) |
N2 | 0.0241 (19) | 0.0186 (18) | 0.0164 (16) | −0.0051 (14) | 0.0065 (14) | 0.0011 (14) |
N3 | 0.0199 (19) | 0.0169 (18) | 0.0149 (17) | −0.0063 (14) | 0.0055 (14) | 0.0017 (13) |
N4 | 0.0207 (19) | 0.0212 (18) | 0.0115 (17) | −0.0002 (14) | −0.0001 (14) | 0.0037 (13) |
C2 | 0.011 (2) | 0.021 (2) | 0.015 (2) | −0.0036 (16) | −0.0010 (16) | 0.0026 (17) |
N5 | 0.0219 (18) | 0.0193 (17) | 0.0084 (15) | 0.0050 (14) | 0.0033 (13) | 0.0003 (13) |
N6 | 0.0281 (19) | 0.0146 (17) | 0.0145 (16) | 0.0021 (14) | −0.0020 (14) | −0.0017 (13) |
N7 | 0.024 (2) | 0.0156 (17) | 0.0115 (16) | −0.0044 (14) | −0.0008 (14) | 0.0025 (13) |
N8 | 0.0174 (18) | 0.0161 (17) | 0.0137 (17) | −0.0036 (14) | −0.0002 (14) | −0.0010 (13) |
C3 | 0.019 (2) | 0.019 (2) | 0.020 (2) | −0.0001 (17) | −0.0007 (16) | −0.0051 (17) |
N9 | 0.028 (2) | 0.0199 (18) | 0.0158 (17) | 0.0072 (15) | 0.0067 (15) | −0.0027 (13) |
N10 | 0.036 (2) | 0.022 (2) | 0.0159 (17) | 0.0115 (16) | 0.0067 (15) | 0.0040 (14) |
N11 | 0.0217 (19) | 0.0129 (17) | 0.0178 (17) | 0.0014 (14) | 0.0032 (14) | 0.0012 (13) |
N12 | 0.033 (2) | 0.0165 (17) | 0.0179 (18) | 0.0004 (15) | 0.0070 (15) | 0.0041 (14) |
C4 | 0.024 (3) | 0.036 (3) | 0.059 (4) | −0.011 (2) | −0.016 (3) | 0.023 (3) |
N13 | 0.032 (2) | 0.0149 (17) | 0.0177 (17) | 0.0069 (15) | 0.0073 (15) | 0.0019 (14) |
N14 | 0.051 (3) | 0.026 (2) | 0.056 (3) | 0.024 (2) | 0.037 (2) | 0.015 (2) |
N151 | 0.021 (2) | 0.016 (2) | 0.022 (2) | 0.0017 (18) | 0.0064 (18) | 0.0023 (18) |
N152 | 0.016 (7) | 0.024 (7) | 0.021 (7) | −0.012 (6) | 0.000 (5) | −0.002 (6) |
N16 | 0.033 (2) | 0.028 (2) | 0.032 (2) | −0.0041 (17) | −0.0065 (17) | 0.0057 (17) |
Geometric parameters (Å, º) top
Sb1—Cl1 | 2.4633 (11) | N6—H61 | 0.9001 |
Sb1—Cl2 | 2.9108 (11) | N6—H62 | 0.9000 |
Sb1—Cl3 | 2.5067 (12) | N7—H7 | 0.9000 |
Sb1—Cl4 | 2.8253 (13) | N8—H81 | 0.9000 |
Sb1—Cl5 | 2.5472 (13) | N8—H82 | 0.9000 |
Sb1—Cl6 | 2.7405 (13) | N8—H83 | 0.9000 |
Sb2—Cl7 | 2.4511 (12) | C3—N9 | 1.311 (5) |
Sb2—Cl8 | 2.9380 (13) | C3—N10 | 1.328 (5) |
Sb2—Cl9 | 2.4508 (11) | C3—N11 | 1.341 (6) |
Sb2—Cl10 | 2.8995 (12) | N11—N12 | 1.408 (5) |
Sb2—Cl11 | 2.4888 (12) | N9—H91 | 0.9001 |
Sb2—Cl12 | 2.8379 (12) | N9—H92 | 0.9000 |
C1—N1 | 1.314 (5) | N10—H101 | 0.9001 |
C1—N2 | 1.316 (5) | N10—H102 | 0.9000 |
C1—N3 | 1.356 (5) | N11—H111 | 0.9001 |
N3—N4 | 1.421 (5) | N12—H121 | 0.9000 |
N1—H11 | 0.8999 | N12—H122 | 0.9000 |
N1—H12 | 0.9000 | C4—N13 | 1.276 (6) |
N2—H21 | 0.9001 | C4—N14 | 1.497 (8) |
N2—H22 | 0.9000 | C4—N152 | 1.055 (15) |
N3—H3 | 0.8999 | C4—N151 | 1.249 (7) |
N4—H41 | 0.9000 | N151—N16 | 1.330 (6) |
N4—H42 | 0.9000 | N13—H131 | 0.9000 |
N4—H43 | 0.9000 | N13—H132 | 0.9000 |
C2—N5 | 1.303 (5) | N14—H141 | 0.9001 |
C2—N6 | 1.312 (5) | N14—H142 | 0.9000 |
C2—N7 | 1.369 (5) | N151—H151 | 0.9000 |
N7—N8 | 1.429 (5) | N152—H152 | 0.9001 |
N5—H51 | 0.8999 | N16—H161 | 0.9000 |
N5—H52 | 0.8999 | N16—H162 | 0.9000 |
| | | |
Cl1—Sb1—Cl2 | 173.85 (4) | N5—C2—N7 | 120.7 (4) |
Cl1—Sb1—Cl3 | 92.89 (4) | N6—C2—N7 | 116.8 (4) |
Cl1—Sb1—Cl4 | 92.07 (4) | N7—N8—H81 | 112.0 |
Cl1—Sb1—Cl5 | 91.35 (4) | N7—N8—H82 | 115.3 |
Cl1—Sb1—Cl6 | 91.70 (4) | N7—N8—H83 | 114.5 |
Cl2—Sb1—Cl3 | 90.06 (4) | N8—N7—H7 | 103.6 |
Cl2—Sb1—Cl4 | 84.85 (3) | N9—C3—N10 | 121.8 (4) |
Cl2—Sb1—Cl5 | 93.95 (3) | N9—C3—N11 | 120.2 (4) |
Cl2—Sb1—Cl6 | 83.00 (3) | N10—C3—N11 | 118.1 (4) |
Cl3—Sb1—Cl4 | 174.79 (3) | H51—N5—H52 | 120.0 |
Cl3—Sb1—Cl5 | 91.69 (4) | H61—N6—H62 | 120.2 |
Cl3—Sb1—Cl6 | 88.18 (4) | H81—N8—H82 | 97.2 |
Cl4—Sb1—Cl5 | 89.78 (4) | H81—N8—H83 | 106.5 |
Cl4—Sb1—Cl6 | 90.09 (4) | H82—N8—H83 | 109.7 |
Cl5—Sb1—Cl6 | 176.95 (3) | C3—N9—H91 | 121.9 |
Cl7—Sb2—Cl8 | 177.50 (3) | C3—N9—H92 | 114.7 |
Cl7—Sb2—Cl9 | 90.08 (4) | C3—N10—H101 | 115.2 |
Cl7—Sb2—Cl10 | 83.03 (3) | C3—N10—H102 | 115.4 |
Cl7—Sb2—Cl11 | 92.50 (4) | C3—N11—N12 | 118.4 (4) |
Cl7—Sb2—Cl12 | 85.21 (4) | C3—N11—H111 | 111.3 |
Cl8—Sb2—Cl9 | 87.49 (4) | N11—N12—H121 | 116.8 |
Cl8—Sb2—Cl10 | 99.28 (3) | N11—N12—H122 | 109.9 |
Cl8—Sb2—Cl11 | 86.89 (4) | N12—N11—H111 | 129.3 |
Cl8—Sb2—Cl12 | 95.68 (3) | H91—N9—H92 | 121.5 |
Cl9—Sb2—Cl10 | 168.90 (4) | H101—N10—H102 | 126.9 |
Cl9—Sb2—Cl11 | 89.08 (4) | H121—N12—H122 | 96.6 |
Cl9—Sb2—Cl12 | 97.76 (4) | C4—N13—H131 | 120.1 |
Cl10—Sb2—Cl11 | 82.56 (3) | C4—N13—H132 | 119.9 |
Cl10—Sb2—Cl12 | 90.35 (3) | C4—N14—H141 | 120.0 |
Cl11—Sb2—Cl12 | 172.78 (3) | C4—N14—H142 | 120.0 |
C1—N1—H11 | 117.0 | C4—N151—N16 | 115.2 (5) |
C1—N1—H12 | 127.2 | C4—N151—H151 | 122.5 |
C1—N2—H21 | 116.4 | C4—N152—N14 | 82.7 (11) |
C1—N2—H22 | 119.9 | C4—N152—H142 | 123.8 |
C1—N3—N4 | 119.0 (3) | C4—N152—H152 | 151.0 |
C1—N3—H3 | 120.0 | N13—C4—N14 | 115.8 (5) |
N1—C1—N2 | 121.5 (4) | N14—N152—H142 | 41.5 |
N1—C1—N3 | 121.6 (4) | N14—N152—H152 | 68.3 |
N2—C1—N3 | 116.9 (4) | N151—C4—N13 | 127.1 (6) |
N3—N4—H41 | 109.1 | N151—C4—N14 | 117.0 (5) |
N3—N4—H42 | 105.7 | N151—N16—H161 | 120.3 |
N3—N4—H43 | 126.2 | N151—N16—H162 | 120.7 |
N4—N3—H3 | 112.1 | N152—C4—N13 | 167.0 (10) |
H11—N1—H12 | 115.8 | N152—C4—N14 | 53.0 (9) |
H21—N2—H22 | 123.6 | N152—N14—C4 | 44.3 (7) |
H41—N4—H42 | 110.3 | N152—N14—H141 | 163.1 |
H41—N4—H43 | 89.1 | N152—N14—H142 | 76.0 |
H42—N4—H43 | 114.6 | N152—N14—H152 | 43.8 |
C2—N5—H51 | 118.2 | N16—N151—H151 | 122.3 |
C2—N5—H52 | 121.8 | H131—N13—H132 | 120.0 |
C2—N6—H61 | 114.2 | H141—N14—H142 | 120.0 |
C2—N6—H62 | 124.1 | H141—N14—H152 | 150.6 |
C2—N7—N8 | 117.7 (3) | H142—N14—H152 | 32.9 |
C2—N7—H7 | 117.8 | H142—N152—H152 | 27.6 |
N5—C2—N6 | 122.4 (4) | H161—N16—H162 | 118.8 |
| | | |
N1—C1—N3—N4 | 15.4 (6) | N10—C3—N11—N12 | 177.2 (4) |
N2—C1—N3—N4 | −166.3 (4) | N13—C4—N14—N152 | −172.2 (10) |
N5—C2—N7—N8 | −39.0 (5) | N13—C4—N151—N16 | −1.4 (8) |
N6—C2—N7—N8 | 145.2 (4) | N14—C4—N151—N16 | −178.4 (4) |
N9—C3—N11—N12 | −2.5 (6) | N13—C4—N152—N14 | 33 (4) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H12···Cl4i | 0.90 | 2.40 | 3.300 (4) | 176 |
N1—H11···Cl10ii | 0.90 | 2.46 | 3.279 (3) | 152 |
N2—H22···Cl12 | 0.90 | 2.45 | 3.267 (3) | 151 |
N2—H21···Cl10ii | 0.90 | 2.44 | 3.255 (3) | 151 |
N4—H41···Cl2i | 0.90 | 2.26 | 3.129 (4) | 164 |
N4—H42···Cl5 | 0.90 | 2.35 | 3.152 (4) | 148 |
N5—H52···Cl8 | 0.90 | 2.31 | 3.192 (3) | 168 |
N5—H51···Cl2iii | 0.90 | 2.44 | 3.269 (3) | 153 |
N6—H62···Cl6 | 0.90 | 2.33 | 3.206 (4) | 166 |
N7—H7···Cl2 | 0.90 | 2.42 | 3.172 (4) | 142 |
N8—H83···Cl8 | 0.90 | 2.27 | 3.100 (4) | 153 |
N8—H82···Cl12 | 0.90 | 2.33 | 3.176 (4) | 157 |
N8—H81···Cl10iv | 0.90 | 2.51 | 3.270 (4) | 142 |
N11—H111···Cl4v | 0.90 | 2.49 | 3.353 (4) | 160 |
Symmetry codes: (i) x−1, y, z; (ii) x, −y+1, z+1/2; (iii) x, −y+1, z−1/2; (iv) x+1, y, z; (v) x, −y, z−1/2. |