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The crystal and molecular structure of the title compound, (CH7N4)(CH8N4)[SbCl6], has been determined at 295 and 92 K. It is composed of isolated [SbCl6]3− octahedra and amino­guanidinium mono- and dications. One of four of the crystallographically inequivalent amino­guanidinium cations is disordered at both temperatures. Two crystallographically inequivalent [SbCl6]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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270101000774/bj1014sup1.cif
Contains datablocks global, Iat295K, Iat92K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101000774/bj1014Iat295Ksup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270101000774/bj1014Iat92Ksup3.hkl
Contains datablock 2

CCDC references: 163896; 163897

Computing details top

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 = 485.67Dx = 1.998 Mg m3
Dm = 1.99 (1) Mg m3
Dm measured by flotation method
Monoclinic, PcMo Kα radiation, λ = 0.71073 Å
a = 7.522 (2) ÅCell parameters from 40 reflections
b = 13.856 (3) Åθ = 7–14°
c = 15.544 (3) ŵ = 2.70 mm1
β = 94.75 (3)°T = 295 K
V = 1614.5 (6) Å3Irregular, colourless
Z = 40.40 × 0.40 × 0.30 mm
Data collection top
KM–4 Diffractometer5052 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 25.1°, θmin = 1.5°
ωθ scanh = 88
Absorption correction: ψ scan
(Sheldrick, 1990)
k = 016
Tmin = 0.446, Tmax = 0.368l = 1818
5690 measured reflections2 standard reflections every 50 reflections
5690 independent reflections intensity decay: 1.0%
Refinement top
Refinement on F2Hydrogen site location: difference Fourier map
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.024Weighting 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 = 1.10Δρmax = 0.59 e Å3
5690 reflectionsΔρmin = 0.36 e Å3
329 parametersExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
40 restraintsExtinction coefficient: 0.0045 (2)
Primary atom site location: PattersonAbsolute structure: (Flack, 1983)
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.04 (2)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sb10.22309 (4)0.24869 (2)0.49848 (2)0.03317 (13)
Cl10.1821 (3)0.08653 (10)0.43411 (11)0.0543 (4)
Cl20.3160 (2)0.43664 (9)0.57138 (9)0.0443 (3)
Cl30.0196 (2)0.32372 (12)0.39736 (10)0.0528 (4)
Cl40.5004 (2)0.18271 (11)0.61516 (11)0.0561 (4)
Cl50.0012 (2)0.21192 (12)0.61079 (11)0.0572 (4)
Cl60.4618 (2)0.29880 (10)0.38538 (10)0.0488 (3)
Sb20.22441 (3)0.73957 (2)0.50076 (2)0.03493 (12)
Cl70.4371 (2)0.69473 (12)0.60557 (10)0.0516 (4)
Cl80.0259 (2)0.79332 (12)0.37415 (11)0.0563 (4)
Cl90.1997 (3)0.90379 (11)0.56122 (11)0.0600 (4)
Cl100.3125 (3)0.55414 (10)0.42616 (11)0.0577 (4)
Cl110.4689 (2)0.79739 (11)0.39258 (10)0.0513 (4)
Cl120.0389 (2)0.65268 (10)0.61370 (9)0.0463 (3)
C10.2310 (8)0.4387 (4)0.6934 (4)0.0360 (12)
N10.3051 (7)0.3636 (3)0.7257 (3)0.0458 (11)
H110.31360.36150.78300.130 (8)*
H120.34890.31390.69310.130 (8)*
N20.1768 (7)0.5132 (4)0.7412 (3)0.0581 (13)
H210.19300.51400.79790.130 (8)*
H220.12250.56310.71710.130 (8)*
N30.2013 (8)0.4434 (3)0.6089 (3)0.0460 (12)
H30.13940.49270.58830.086 (13)*
N40.2817 (7)0.3757 (3)0.5513 (3)0.0438 (11)
H410.40160.37800.54800.092 (9)*
H420.24930.31400.56180.092 (9)*
H430.24810.39100.49880.092 (9)*
C20.2508 (8)0.5506 (4)0.3070 (4)0.0393 (13)
N50.2289 (7)0.6344 (3)0.2663 (3)0.0496 (13)
H510.29090.64330.21980.130 (8)*
H520.19150.68610.29490.130 (8)*
N60.2923 (7)0.4736 (3)0.2672 (3)0.0583 (14)
H610.25440.47670.21080.130 (8)*
H620.30890.41440.29030.130 (8)*
N70.2234 (8)0.5448 (3)0.3917 (3)0.0508 (14)
H70.23790.48820.41980.086 (13)*
N80.2633 (7)0.6232 (4)0.4478 (3)0.0461 (12)
H810.38020.63730.44830.092 (9)*
H820.23710.60720.50140.092 (9)*
H830.19840.67490.42950.092 (9)*
C30.2761 (10)0.0548 (5)0.1938 (5)0.0557 (17)
N90.2177 (9)0.1381 (4)0.2192 (4)0.0682 (17)
H910.23370.14140.27710.130 (8)*
H920.20330.19680.19470.130 (8)*
N100.3041 (9)0.0206 (4)0.2491 (4)0.0809 (19)
H1010.28490.01340.30510.130 (8)*
H1020.34350.07740.23000.130 (8)*
N110.3025 (9)0.0415 (4)0.1129 (4)0.0647 (16)
H1110.32320.02140.10370.086 (13)*
N120.2686 (9)0.1151 (4)0.0566 (4)0.0657 (16)
H1210.17940.10160.01610.130 (8)*
H1220.35920.13390.02610.130 (8)*
C410.2711 (18)1.0688 (10)0.3362 (9)0.042 (3)0.60
C420.241 (3)1.0438 (16)0.3047 (16)0.046 (5)0.40
N130.2870 (10)1.1308 (4)0.2751 (4)0.079 (2)
H1310.31881.19220.28490.130 (8)*
H1320.26531.11210.22150.130 (8)*
N140.3009 (10)1.0930 (5)0.4250 (5)0.092 (2)
H1410.33811.15240.43840.130 (8)*
H1420.28361.04780.46640.130 (8)*
N1510.2162 (12)0.9813 (7)0.3195 (6)0.054 (2)0.60
H1510.20310.93560.36070.086 (13)*0.60
N1520.249 (2)1.0244 (10)0.3831 (9)0.055 (3)0.40
H1520.21850.96640.40570.086 (13)*0.40
N160.1830 (9)0.9632 (4)0.2420 (4)0.0782 (18)
H1610.14550.90420.22720.130 (8)*
H1620.19711.01000.20190.130 (8)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.0402 (3)0.03043 (16)0.0289 (2)0.00185 (11)0.0031 (2)0.00077 (13)
Cl10.0807 (12)0.0373 (7)0.0448 (8)0.0031 (7)0.0047 (8)0.0048 (6)
Cl20.0628 (10)0.0387 (6)0.0325 (7)0.0068 (6)0.0099 (6)0.0015 (5)
Cl30.0484 (8)0.0642 (9)0.0448 (8)0.0068 (7)0.0017 (6)0.0127 (7)
Cl40.0579 (10)0.0463 (8)0.0620 (9)0.0079 (7)0.0083 (7)0.0099 (7)
Cl50.0634 (10)0.0610 (9)0.0499 (9)0.0056 (8)0.0210 (7)0.0108 (7)
Cl60.0535 (9)0.0494 (8)0.0445 (8)0.0098 (6)0.0105 (6)0.0026 (6)
Sb20.0385 (3)0.03486 (17)0.0315 (2)0.00055 (17)0.0032 (2)0.00171 (18)
Cl70.0484 (8)0.0656 (9)0.0424 (8)0.0015 (7)0.0136 (6)0.0054 (7)
Cl80.0582 (9)0.0658 (10)0.0460 (8)0.0140 (8)0.0118 (7)0.0062 (7)
Cl90.0869 (13)0.0443 (8)0.0491 (9)0.0063 (8)0.0074 (8)0.0096 (6)
Cl100.0952 (14)0.0413 (7)0.0380 (8)0.0051 (8)0.0149 (8)0.0042 (6)
Cl110.0446 (8)0.0599 (8)0.0478 (8)0.0004 (7)0.0063 (6)0.0144 (7)
Cl120.0431 (7)0.0548 (8)0.0407 (7)0.0007 (6)0.0025 (6)0.0088 (6)
C10.039 (3)0.036 (3)0.032 (3)0.003 (2)0.000 (2)0.008 (2)
N10.057 (3)0.052 (3)0.028 (2)0.010 (2)0.005 (2)0.0036 (19)
N20.082 (4)0.055 (3)0.038 (3)0.023 (3)0.009 (3)0.005 (2)
N30.061 (3)0.045 (3)0.033 (3)0.010 (2)0.012 (2)0.001 (2)
N40.047 (3)0.053 (3)0.031 (3)0.002 (2)0.004 (2)0.008 (2)
C20.043 (3)0.043 (3)0.031 (3)0.004 (2)0.001 (2)0.005 (2)
N50.076 (4)0.045 (3)0.028 (2)0.006 (2)0.004 (2)0.0054 (19)
N60.087 (4)0.043 (3)0.041 (3)0.009 (3)0.011 (3)0.002 (2)
N70.076 (4)0.043 (3)0.032 (3)0.015 (2)0.004 (2)0.009 (2)
N80.055 (3)0.056 (3)0.028 (3)0.008 (2)0.009 (2)0.000 (2)
C30.054 (4)0.067 (4)0.045 (4)0.001 (3)0.001 (3)0.009 (3)
N90.104 (5)0.050 (3)0.049 (3)0.019 (3)0.000 (3)0.010 (2)
N100.119 (6)0.067 (4)0.059 (4)0.032 (4)0.018 (4)0.002 (3)
N110.086 (4)0.051 (3)0.058 (4)0.004 (3)0.013 (3)0.006 (3)
N120.088 (4)0.046 (3)0.064 (4)0.001 (3)0.010 (3)0.004 (3)
C410.044 (7)0.040 (7)0.043 (8)0.008 (5)0.006 (5)0.010 (6)
C420.041 (9)0.036 (11)0.061 (14)0.007 (8)0.011 (9)0.004 (9)
N130.144 (7)0.049 (3)0.046 (3)0.026 (3)0.017 (4)0.013 (3)
N140.122 (6)0.063 (4)0.098 (6)0.040 (4)0.051 (5)0.018 (4)
N1510.069 (6)0.043 (5)0.050 (5)0.009 (4)0.011 (4)0.010 (4)
N1520.087 (10)0.036 (6)0.041 (7)0.002 (6)0.000 (6)0.008 (6)
N160.117 (5)0.057 (3)0.059 (4)0.005 (3)0.002 (4)0.005 (3)
Geometric parameters (Å, º) top
Sb1—Cl12.469 (2)N7—H70.9000
Sb1—Cl22.902 (2)N8—H810.9000
Sb1—Cl32.532 (2)N8—H820.9000
Sb1—Cl42.802 (2)N8—H830.9000
Sb1—Cl52.577 (2)C3—N91.308 (8)
Sb1—Cl62.705 (2)C3—N101.359 (9)
Sb2—Cl72.456 (2)C3—N111.302 (9)
Sb2—Cl82.931 (2)N11—N121.354 (8)
Sb2—Cl92.463 (2)N9—H910.9000
Sb2—Cl102.874 (2)N9—H920.9001
Sb2—Cl112.518 (2)N10—H1010.9000
Sb2—Cl122.807 (2)N10—H1020.9000
C1—N11.301 (7)N11—H1110.9000
C1—N21.316 (7)N12—H1210.9000
C1—N31.352 (7)N12—H1220.9001
N3—N41.399 (7)C41—N131.279 (15)
N1—H110.9000C41—N141.455 (15)
N1—H120.9000C41—N1511.314 (15)
N2—H210.9000C42—N1521.25 (3)
N2—H220.9000C42—N131.33 (2)
N3—H30.9000C42—N161.57 (2)
N4—H410.9000N13—H1310.9000
N4—H420.9000N13—H1320.9000
N4—H430.9000N14—N1521.232 (15)
C2—N51.327 (7)N14—H1410.9000
C2—N61.284 (7)N14—H1420.8999
C2—N71.352 (7)N151—N161.275 (10)
N7—N81.409 (7)N151—H1510.9000
N5—H510.9000N152—H1520.9001
N5—H520.8999N16—H1610.9000
N6—H610.9000N16—H1620.9000
N6—H620.9001
Cl1—Sb1—Cl2173.19 (6)N6—C2—N5121.5 (5)
Cl1—Sb1—Cl393.59 (6)N6—C2—N7118.9 (5)
Cl1—Sb1—Cl491.53 (5)N7—N8—H81109.4
Cl1—Sb1—Cl591.59 (6)N7—N8—H82109.4
Cl1—Sb1—Cl692.15 (6)N7—N8—H83109.7
Cl2—Sb1—Cl390.68 (5)N8—N7—H7111.1
Cl2—Sb1—Cl484.13 (5)H51—N5—H52119.5
Cl2—Sb1—Cl593.61 (5)H61—N6—H62117.0
Cl2—Sb1—Cl682.65 (5)H81—N8—H82109.5
Cl3—Sb1—Cl4174.79 (5)H81—N8—H83109.5
Cl3—Sb1—Cl591.31 (6)H82—N8—H83109.5
Cl3—Sb1—Cl688.54 (5)C3—N9—H91109.0
Cl4—Sb1—Cl589.49 (6)C3—N9—H92134.5
Cl4—Sb1—Cl690.33 (5)C3—N10—H101119.9
Cl5—Sb1—Cl6176.25 (5)C3—N10—H102120.1
Cl7—Sb2—Cl8179.34 (5)C3—N11—N12118.9 (6)
Cl7—Sb2—Cl990.77 (6)C3—N11—H111109.4
Cl7—Sb2—Cl1084.28 (5)N9—C3—N10121.7 (6)
Cl7—Sb2—Cl1192.51 (6)N11—C3—N9119.9 (7)
Cl7—Sb2—Cl1286.63 (5)N11—C3—N10118.3 (6)
Cl8—Sb2—Cl989.37 (6)N11—N12—H121112.7
Cl8—Sb2—Cl1095.50 (5)N11—N12—H122116.6
Cl8—Sb2—Cl1186.85 (5)N12—N11—H111130.8
Cl8—Sb2—Cl1293.99 (5)H91—N9—H92112.2
Cl9—Sb2—Cl10170.96 (7)H101—N10—H102120.0
Cl9—Sb2—Cl1189.36 (6)H121—N12—H122104.2
Cl9—Sb2—Cl1297.50 (6)C41—N13—H131121.2
Cl10—Sb2—Cl1183.32 (5)C41—N13—H132118.8
Cl10—Sb2—Cl1289.77 (5)C41—N14—H141120.4
Cl11—Sb2—Cl12173.10 (5)C41—N14—H142119.6
C1—N1—H11118.4C41—N151—H151121.8
C1—N1—H12122.9C42—N13—H131149.9
C1—N2—H21120.1C42—N13—H13289.9
C1—N2—H22119.9C42—N152—H152122.6
C1—N3—N4119.5 (5)C42—N16—H161156.1
C1—N3—H3120.9C42—N16—H16283.9
N1—C1—N2122.2 (5)N13—C41—N151119.0 (12)
N1—C1—N3121.5 (5)N13—C41—N14122.5 (10)
N2—C1—N3116.3 (5)N13—C42—N16120.6 (18)
N3—N4—H41113.1N14—N152—C42113.1 (16)
N3—N4—H42115.2N14—N152—H14239.8
N3—N4—H43106.5N14—N152—H152124.3
N4—N3—H3119.3N151—C41—N14118.4 (11)
H11—N1—H12118.7N151—N16—H161120.6
H21—N2—H22120.0N151—N16—H162119.4
H41—N4—H42107.4N152—C42—N13120.0 (18)
H41—N4—H43107.1N152—C42—N16119.4 (19)
H42—N4—H43107.2N152—N14—H141161.0
C2—N5—H51116.7N152—N14—H14279.0
C2—N5—H52119.5N16—N151—C41117.2 (10)
C2—N6—H61111.1N16—N151—H151121.0
C2—N6—H62126.5H131—N13—H132120.0
C2—N7—N8121.0 (5)H141—N14—H142120.0
C2—N7—H7120.1H142—N152—H15284.5
N5—C2—N7119.5 (5)H161—N16—H162120.0
N1—C1—N3—N412.7 (9)N10—C3—N11—N12177.5 (7)
N2—C1—N3—N4169.0 (5)N13—C41—N151—N160.5 (18)
N6—C2—N7—N8148.7 (6)N14—C41—N151—N16176.8 (9)
N5—C2—N7—N833.4 (9)N13—C42—N152—N140 (3)
N9—C3—N11—N120.0 (11)N16—C42—N152—N14178.3 (14)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H12···Cl4i0.902.413.310 (5)173
N1—H11···Cl10ii0.902.513.323 (5)150
N2—H22···Cl120.902.433.291 (5)159
N2—H21···Cl10ii0.902.443.266 (5)152
N4—H41···Cl2i0.902.333.182 (5)158
N4—H42···Cl50.902.413.183 (5)144
N5—H52···Cl80.902.353.227 (5)164
N5—H51···Cl2iii0.902.583.303 (5)138
N6—H62···Cl60.902.413.238 (5)154
N7—H7···Cl20.902.493.195 (5)136
N8—H83···Cl80.902.223.118 (6)174
N8—H82···Cl120.902.473.223 (5)142
N8—H81···Cl10iv0.902.633.374 (6)141
N11—H111···Cl4v0.902.603.444 (6)157
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z+1/2; (iii) x, y+1, z1/2; (iv) x+1, y, z; (v) x, y, z1/2.
(Iat92K) Aminoguanidinium(1+)(2+) heksachloroantimonate(III) top
Crystal data top
(CH7N4)(CH8N4)[SbCl6]F(000) = 944
Mr = 485.67Dx = 2.047 Mg m3
Monoclinic, PcMo Kα radiation, λ = 0.71073 Å
a = 7.426 (2) ÅCell parameters from 40 reflections
b = 13.836 (3) Åθ = 7–14°
c = 15.403 (3) ŵ = 2.76 mm1
β = 95.27 (3)°T = 92 K
V = 1575.9 (6) Å3Irregular, colourless
Z = 40.40 × 0.40 × 0.30 mm
Data collection top
KUMA KM–4 Diffractometer5334 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 25.1°, θmin = 1.5°
ωθ scanh = 88
Absorption correction: ψ scan
(Sheldrick, 1990)
k = 160
Tmin = 0.360, Tmax = 0.437l = 1817
5579 measured reflections2 standard reflections every 50 reflections
5579 independent reflections intensity decay: 1.1%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.019H-atom parameters constrained
wR(F2) = 0.048Weighting 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 reflectionsΔρmax = 0.48 e Å3
319 parametersΔρmin = 0.56 e Å3
27 restraintsAbsolute structure: (Flack, 1983)
Primary atom site location: PattersonAbsolute structure parameter: 0.026 (15)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Sb10.21663 (3)0.24731 (2)0.50009 (2)0.01226 (7)
Cl10.16847 (15)0.08646 (7)0.43343 (7)0.0197 (2)
Cl20.31288 (14)0.43630 (7)0.57333 (6)0.01589 (19)
Cl30.02444 (13)0.32359 (7)0.39779 (6)0.0187 (2)
Cl40.50038 (14)0.17844 (7)0.61877 (7)0.0210 (2)
Cl50.00845 (14)0.21124 (7)0.61105 (7)0.0219 (2)
Cl60.46172 (13)0.29562 (7)0.38473 (6)0.0180 (2)
Sb20.21786 (2)0.73996 (2)0.49897 (1)0.01230 (7)
Cl70.43114 (13)0.69876 (7)0.60558 (6)0.0179 (2)
Cl80.03592 (14)0.79826 (7)0.37311 (7)0.0203 (2)
Cl90.19014 (16)0.90405 (7)0.55862 (7)0.0221 (2)
Cl100.32523 (15)0.55302 (7)0.42652 (7)0.0192 (2)
Cl110.46382 (13)0.79786 (7)0.39081 (6)0.01658 (19)
Cl120.04560 (13)0.65015 (7)0.61760 (6)0.01566 (19)
C10.2339 (6)0.4386 (3)0.6944 (3)0.0145 (8)
N10.3151 (4)0.3646 (2)0.7274 (2)0.0156 (7)
H110.31980.36400.78560.051 (4)*
H120.37060.31510.69800.051 (4)*
N20.1783 (4)0.5131 (2)0.7429 (2)0.0194 (7)
H210.18160.50630.80080.051 (4)*
H220.14120.56730.71760.051 (4)*
N30.1992 (5)0.4407 (2)0.6096 (2)0.0170 (7)
H30.17780.49750.58380.021 (6)*
N40.2892 (5)0.3740 (3)0.5504 (2)0.0179 (8)
H410.40940.38000.55250.039 (6)*
H420.25200.31510.56920.039 (6)*
H430.30540.38020.49200.039 (6)*
C20.2442 (5)0.5527 (3)0.3096 (3)0.0158 (8)
N50.2253 (5)0.6343 (2)0.2676 (2)0.0164 (7)
H510.25720.63660.21270.051 (4)*
H520.17720.68670.29120.051 (4)*
N60.2853 (5)0.4718 (2)0.2716 (2)0.0193 (7)
H610.25520.47070.21360.051 (4)*
H620.31610.41680.30040.051 (4)*
N70.2093 (5)0.5466 (2)0.3952 (2)0.0172 (7)
H70.25100.49460.42580.021 (6)*
N80.2636 (5)0.6259 (2)0.4510 (2)0.0159 (7)
H810.38370.62620.46580.039 (6)*
H820.22900.62220.50530.039 (6)*
H830.23550.68450.42820.039 (6)*
C30.2785 (6)0.0559 (3)0.1963 (3)0.0193 (9)
N90.2154 (5)0.1391 (3)0.2207 (2)0.0209 (8)
H910.20560.15300.27710.051 (4)*
H920.21120.18560.17980.051 (4)*
N100.3108 (5)0.0167 (3)0.2520 (2)0.0246 (8)
H1010.30220.00180.30830.051 (4)*
H1020.36840.06780.23130.051 (4)*
N110.3114 (5)0.0419 (3)0.1131 (2)0.0174 (7)
H1110.33970.02020.10330.021 (6)*
N120.2699 (5)0.1169 (2)0.0527 (2)0.0222 (8)
H1210.18630.10400.00820.051 (4)*
H1220.36290.12620.02010.051 (4)*
C40.2714 (7)1.0646 (4)0.3292 (4)0.0408 (15)
N130.2955 (5)1.1322 (2)0.2730 (2)0.0213 (8)
H1310.33641.19030.28870.051 (4)*
H1320.27111.12180.21760.051 (4)*
N140.3162 (6)1.0891 (3)0.4194 (3)0.0425 (13)
H1410.35671.14860.43120.051 (4)*
H1420.30261.04430.46190.051 (4)*
N1510.2085 (6)0.9824 (3)0.3178 (3)0.0193 (9)0.75
H1510.19320.93830.36080.021 (6)*0.75
N1520.2463 (18)1.0219 (11)0.3857 (9)0.020 (3)0.25
H1520.25001.01280.44340.021 (6)*0.25
N160.1662 (5)0.9643 (3)0.2374 (2)0.0317 (9)
H1610.04990.95720.22660.051 (4)*
H1620.25330.95480.19360.051 (4)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Sb10.01483 (15)0.01068 (12)0.01142 (14)0.00152 (9)0.00200 (12)0.00028 (9)
Cl10.0291 (6)0.0134 (4)0.0170 (5)0.0010 (4)0.0035 (4)0.0016 (4)
Cl20.0215 (5)0.0151 (4)0.0115 (4)0.0021 (4)0.0041 (4)0.0010 (3)
Cl30.0179 (5)0.0224 (5)0.0159 (5)0.0029 (4)0.0017 (4)0.0046 (4)
Cl40.0217 (5)0.0158 (5)0.0250 (5)0.0028 (4)0.0005 (4)0.0042 (4)
Cl50.0236 (5)0.0238 (5)0.0196 (5)0.0035 (4)0.0089 (4)0.0044 (4)
Cl60.0205 (5)0.0167 (5)0.0175 (5)0.0039 (4)0.0059 (4)0.0005 (4)
Sb20.01313 (14)0.01184 (12)0.01204 (14)0.00000 (11)0.00177 (12)0.00080 (11)
Cl70.0156 (5)0.0238 (5)0.0148 (5)0.0017 (4)0.0040 (4)0.0013 (4)
Cl80.0200 (5)0.0261 (5)0.0152 (5)0.0055 (4)0.0044 (4)0.0012 (4)
Cl90.0282 (6)0.0201 (5)0.0182 (5)0.0038 (4)0.0034 (4)0.0042 (4)
Cl100.0243 (5)0.0166 (5)0.0174 (5)0.0044 (4)0.0069 (4)0.0034 (4)
Cl110.0140 (4)0.0189 (5)0.0166 (4)0.0002 (4)0.0002 (3)0.0030 (4)
Cl120.0145 (5)0.0195 (5)0.0133 (4)0.0001 (4)0.0027 (3)0.0031 (4)
C10.014 (2)0.0148 (19)0.0151 (19)0.0010 (16)0.0022 (15)0.0009 (16)
N10.0156 (16)0.0178 (17)0.0138 (16)0.0024 (14)0.0032 (14)0.0016 (13)
N20.0241 (19)0.0186 (18)0.0164 (16)0.0051 (14)0.0065 (14)0.0011 (14)
N30.0199 (19)0.0169 (18)0.0149 (17)0.0063 (14)0.0055 (14)0.0017 (13)
N40.0207 (19)0.0212 (18)0.0115 (17)0.0002 (14)0.0001 (14)0.0037 (13)
C20.011 (2)0.021 (2)0.015 (2)0.0036 (16)0.0010 (16)0.0026 (17)
N50.0219 (18)0.0193 (17)0.0084 (15)0.0050 (14)0.0033 (13)0.0003 (13)
N60.0281 (19)0.0146 (17)0.0145 (16)0.0021 (14)0.0020 (14)0.0017 (13)
N70.024 (2)0.0156 (17)0.0115 (16)0.0044 (14)0.0008 (14)0.0025 (13)
N80.0174 (18)0.0161 (17)0.0137 (17)0.0036 (14)0.0002 (14)0.0010 (13)
C30.019 (2)0.019 (2)0.020 (2)0.0001 (17)0.0007 (16)0.0051 (17)
N90.028 (2)0.0199 (18)0.0158 (17)0.0072 (15)0.0067 (15)0.0027 (13)
N100.036 (2)0.022 (2)0.0159 (17)0.0115 (16)0.0067 (15)0.0040 (14)
N110.0217 (19)0.0129 (17)0.0178 (17)0.0014 (14)0.0032 (14)0.0012 (13)
N120.033 (2)0.0165 (17)0.0179 (18)0.0004 (15)0.0070 (15)0.0041 (14)
C40.024 (3)0.036 (3)0.059 (4)0.011 (2)0.016 (3)0.023 (3)
N130.032 (2)0.0149 (17)0.0177 (17)0.0069 (15)0.0073 (15)0.0019 (14)
N140.051 (3)0.026 (2)0.056 (3)0.024 (2)0.037 (2)0.015 (2)
N1510.021 (2)0.016 (2)0.022 (2)0.0017 (18)0.0064 (18)0.0023 (18)
N1520.016 (7)0.024 (7)0.021 (7)0.012 (6)0.000 (5)0.002 (6)
N160.033 (2)0.028 (2)0.032 (2)0.0041 (17)0.0065 (17)0.0057 (17)
Geometric parameters (Å, º) top
Sb1—Cl12.4633 (11)N6—H610.9001
Sb1—Cl22.9108 (11)N6—H620.9000
Sb1—Cl32.5067 (12)N7—H70.9000
Sb1—Cl42.8253 (13)N8—H810.9000
Sb1—Cl52.5472 (13)N8—H820.9000
Sb1—Cl62.7405 (13)N8—H830.9000
Sb2—Cl72.4511 (12)C3—N91.311 (5)
Sb2—Cl82.9380 (13)C3—N101.328 (5)
Sb2—Cl92.4508 (11)C3—N111.341 (6)
Sb2—Cl102.8995 (12)N11—N121.408 (5)
Sb2—Cl112.4888 (12)N9—H910.9001
Sb2—Cl122.8379 (12)N9—H920.9000
C1—N11.314 (5)N10—H1010.9001
C1—N21.316 (5)N10—H1020.9000
C1—N31.356 (5)N11—H1110.9001
N3—N41.421 (5)N12—H1210.9000
N1—H110.8999N12—H1220.9000
N1—H120.9000C4—N131.276 (6)
N2—H210.9001C4—N141.497 (8)
N2—H220.9000C4—N1521.055 (15)
N3—H30.8999C4—N1511.249 (7)
N4—H410.9000N151—N161.330 (6)
N4—H420.9000N13—H1310.9000
N4—H430.9000N13—H1320.9000
C2—N51.303 (5)N14—H1410.9001
C2—N61.312 (5)N14—H1420.9000
C2—N71.369 (5)N151—H1510.9000
N7—N81.429 (5)N152—H1520.9001
N5—H510.8999N16—H1610.9000
N5—H520.8999N16—H1620.9000
Cl1—Sb1—Cl2173.85 (4)N5—C2—N7120.7 (4)
Cl1—Sb1—Cl392.89 (4)N6—C2—N7116.8 (4)
Cl1—Sb1—Cl492.07 (4)N7—N8—H81112.0
Cl1—Sb1—Cl591.35 (4)N7—N8—H82115.3
Cl1—Sb1—Cl691.70 (4)N7—N8—H83114.5
Cl2—Sb1—Cl390.06 (4)N8—N7—H7103.6
Cl2—Sb1—Cl484.85 (3)N9—C3—N10121.8 (4)
Cl2—Sb1—Cl593.95 (3)N9—C3—N11120.2 (4)
Cl2—Sb1—Cl683.00 (3)N10—C3—N11118.1 (4)
Cl3—Sb1—Cl4174.79 (3)H51—N5—H52120.0
Cl3—Sb1—Cl591.69 (4)H61—N6—H62120.2
Cl3—Sb1—Cl688.18 (4)H81—N8—H8297.2
Cl4—Sb1—Cl589.78 (4)H81—N8—H83106.5
Cl4—Sb1—Cl690.09 (4)H82—N8—H83109.7
Cl5—Sb1—Cl6176.95 (3)C3—N9—H91121.9
Cl7—Sb2—Cl8177.50 (3)C3—N9—H92114.7
Cl7—Sb2—Cl990.08 (4)C3—N10—H101115.2
Cl7—Sb2—Cl1083.03 (3)C3—N10—H102115.4
Cl7—Sb2—Cl1192.50 (4)C3—N11—N12118.4 (4)
Cl7—Sb2—Cl1285.21 (4)C3—N11—H111111.3
Cl8—Sb2—Cl987.49 (4)N11—N12—H121116.8
Cl8—Sb2—Cl1099.28 (3)N11—N12—H122109.9
Cl8—Sb2—Cl1186.89 (4)N12—N11—H111129.3
Cl8—Sb2—Cl1295.68 (3)H91—N9—H92121.5
Cl9—Sb2—Cl10168.90 (4)H101—N10—H102126.9
Cl9—Sb2—Cl1189.08 (4)H121—N12—H12296.6
Cl9—Sb2—Cl1297.76 (4)C4—N13—H131120.1
Cl10—Sb2—Cl1182.56 (3)C4—N13—H132119.9
Cl10—Sb2—Cl1290.35 (3)C4—N14—H141120.0
Cl11—Sb2—Cl12172.78 (3)C4—N14—H142120.0
C1—N1—H11117.0C4—N151—N16115.2 (5)
C1—N1—H12127.2C4—N151—H151122.5
C1—N2—H21116.4C4—N152—N1482.7 (11)
C1—N2—H22119.9C4—N152—H142123.8
C1—N3—N4119.0 (3)C4—N152—H152151.0
C1—N3—H3120.0N13—C4—N14115.8 (5)
N1—C1—N2121.5 (4)N14—N152—H14241.5
N1—C1—N3121.6 (4)N14—N152—H15268.3
N2—C1—N3116.9 (4)N151—C4—N13127.1 (6)
N3—N4—H41109.1N151—C4—N14117.0 (5)
N3—N4—H42105.7N151—N16—H161120.3
N3—N4—H43126.2N151—N16—H162120.7
N4—N3—H3112.1N152—C4—N13167.0 (10)
H11—N1—H12115.8N152—C4—N1453.0 (9)
H21—N2—H22123.6N152—N14—C444.3 (7)
H41—N4—H42110.3N152—N14—H141163.1
H41—N4—H4389.1N152—N14—H14276.0
H42—N4—H43114.6N152—N14—H15243.8
C2—N5—H51118.2N16—N151—H151122.3
C2—N5—H52121.8H131—N13—H132120.0
C2—N6—H61114.2H141—N14—H142120.0
C2—N6—H62124.1H141—N14—H152150.6
C2—N7—N8117.7 (3)H142—N14—H15232.9
C2—N7—H7117.8H142—N152—H15227.6
N5—C2—N6122.4 (4)H161—N16—H162118.8
N1—C1—N3—N415.4 (6)N10—C3—N11—N12177.2 (4)
N2—C1—N3—N4166.3 (4)N13—C4—N14—N152172.2 (10)
N5—C2—N7—N839.0 (5)N13—C4—N151—N161.4 (8)
N6—C2—N7—N8145.2 (4)N14—C4—N151—N16178.4 (4)
N9—C3—N11—N122.5 (6)N13—C4—N152—N1433 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H12···Cl4i0.902.403.300 (4)176
N1—H11···Cl10ii0.902.463.279 (3)152
N2—H22···Cl120.902.453.267 (3)151
N2—H21···Cl10ii0.902.443.255 (3)151
N4—H41···Cl2i0.902.263.129 (4)164
N4—H42···Cl50.902.353.152 (4)148
N5—H52···Cl80.902.313.192 (3)168
N5—H51···Cl2iii0.902.443.269 (3)153
N6—H62···Cl60.902.333.206 (4)166
N7—H7···Cl20.902.423.172 (4)142
N8—H83···Cl80.902.273.100 (4)153
N8—H82···Cl120.902.333.176 (4)157
N8—H81···Cl10iv0.902.513.270 (4)142
N11—H111···Cl4v0.902.493.353 (4)160
Symmetry codes: (i) x1, y, z; (ii) x, y+1, z+1/2; (iii) x, y+1, z1/2; (iv) x+1, y, z; (v) x, y, z1/2.
 

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