Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S205322961700314X/ky3114sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961700314X/ky3114Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961700314X/ky3114IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961700314X/ky3114IIIsup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S205322961700314X/ky3114IVsup5.hkl | |
Chemical Markup Language (CML) file https://doi.org/10.1107/S205322961700314X/ky3114Isup6.cml |
CCDC references: 1534722; 1534721; 1534720; 1534719
For all compounds, data collection: CrysAlis PRO (Rigaku OD, 2015); cell refinement: CrysAlis PRO (Rigaku OD, 2015); data reduction: CrysAlis PRO (Rigaku OD, 2015). Program(s) used to solve structure: SIR 92 (Altomare et al., 1993) for (I); SHELXS97 (Sheldrick, 2008) for (II), (III); SIR92 (Altomare et al., 1993) for (IV). For all compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009).
C6H9AsNO3+·Cl− | F(000) = 504 |
Mr = 253.51 | Dx = 1.810 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 1528 reflections |
a = 16.6534 (8) Å | θ = 4.4–29.2° |
b = 7.4129 (3) Å | µ = 3.91 mm−1 |
c = 7.6073 (4) Å | T = 200 K |
β = 97.795 (4)° | Plate, colourless |
V = 930.44 (8) Å3 | 0.40 × 0.40 × 0.15 mm |
Z = 4 |
Oxford Diffraction Gemini-S CCD-detector diffractometer | 1820 independent reflections |
Radiation source: Enhance (Mo) X-ray source | 1601 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
Detector resolution: 16.077 pixels mm-1 | θmax = 26.0°, θmin = 3.7° |
ω scans | h = −20→9 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015) | k = −8→9 |
Tmin = 0.66, Tmax = 0.98 | l = −9→9 |
3922 measured reflections |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.068 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0304P)2 + 0.3689P] where P = (Fo2 + 2Fc2)/3 |
1820 reflections | (Δ/σ)max = 0.001 |
124 parameters | Δρmax = 0.44 e Å−3 |
5 restraints | Δρmin = −0.48 e Å−3 |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles |
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 > 2sigma(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 | ||
As1 | 0.37111 (2) | 0.53013 (4) | 0.52946 (4) | 0.0235 (1) | |
O11 | 0.43235 (13) | 0.4083 (3) | 0.6799 (3) | 0.0387 (8) | |
O12 | 0.41875 (13) | 0.6107 (3) | 0.3702 (3) | 0.0345 (7) | |
O13 | 0.32856 (15) | 0.6985 (3) | 0.6375 (3) | 0.0454 (8) | |
N4 | 0.08067 (16) | 0.0693 (3) | 0.2459 (3) | 0.0218 (8) | |
C1 | 0.28113 (17) | 0.3841 (4) | 0.4442 (3) | 0.0200 (8) | |
C2 | 0.28676 (18) | 0.1973 (4) | 0.4548 (4) | 0.0263 (9) | |
C3 | 0.22080 (19) | 0.0936 (4) | 0.3897 (4) | 0.0252 (9) | |
C4 | 0.15124 (17) | 0.1775 (3) | 0.3126 (3) | 0.0178 (8) | |
C5 | 0.14488 (18) | 0.3635 (3) | 0.2991 (4) | 0.0225 (8) | |
C6 | 0.21088 (18) | 0.4666 (4) | 0.3665 (4) | 0.0246 (9) | |
Cl1 | 0.05319 (5) | −0.22825 (9) | 0.51606 (9) | 0.0245 (2) | |
H2 | 0.33570 | 0.14160 | 0.50660 | 0.0310* | |
H3 | 0.22330 | −0.03420 | 0.39800 | 0.0300* | |
H5 | 0.09630 | 0.41860 | 0.24480 | 0.0270* | |
H6 | 0.20800 | 0.59440 | 0.35950 | 0.0300* | |
H11 | 0.4836 (13) | 0.400 (5) | 0.664 (5) | 0.0580* | |
H13 | 0.363 (2) | 0.748 (5) | 0.720 (4) | 0.0680* | |
H41 | 0.090 (2) | −0.014 (3) | 0.171 (3) | 0.0260* | |
H42 | 0.0631 (19) | 0.008 (3) | 0.330 (3) | 0.0260* | |
H43 | 0.0432 (15) | 0.135 (3) | 0.185 (3) | 0.0260* |
U11 | U22 | U33 | U12 | U13 | U23 | |
As1 | 0.0114 (2) | 0.0300 (2) | 0.0279 (2) | −0.0011 (1) | −0.0019 (1) | −0.0005 (1) |
O11 | 0.0152 (12) | 0.0649 (15) | 0.0346 (12) | 0.0039 (11) | −0.0017 (10) | 0.0195 (11) |
O12 | 0.0170 (12) | 0.0419 (12) | 0.0441 (13) | 0.0039 (10) | 0.0024 (10) | 0.0197 (11) |
O13 | 0.0187 (13) | 0.0528 (15) | 0.0621 (16) | −0.0012 (11) | −0.0035 (11) | −0.0324 (13) |
N4 | 0.0249 (15) | 0.0208 (13) | 0.0189 (12) | −0.0069 (11) | 0.0001 (10) | 0.0011 (10) |
C1 | 0.0163 (15) | 0.0247 (14) | 0.0188 (13) | −0.0008 (12) | 0.0015 (11) | −0.0004 (12) |
C2 | 0.0206 (17) | 0.0280 (15) | 0.0297 (15) | 0.0080 (12) | 0.0016 (13) | 0.0041 (13) |
C3 | 0.0295 (18) | 0.0159 (13) | 0.0300 (15) | 0.0026 (12) | 0.0037 (13) | 0.0018 (12) |
C4 | 0.0200 (15) | 0.0188 (13) | 0.0146 (12) | −0.0040 (11) | 0.0027 (11) | −0.0026 (11) |
C5 | 0.0180 (15) | 0.0214 (14) | 0.0261 (14) | 0.0030 (12) | −0.0039 (12) | 0.0027 (12) |
C6 | 0.0186 (16) | 0.0177 (13) | 0.0363 (16) | −0.0016 (12) | −0.0005 (13) | −0.0016 (12) |
Cl1 | 0.0315 (4) | 0.0200 (3) | 0.0212 (3) | 0.0009 (3) | 0.0009 (3) | 0.0032 (3) |
As1—O11 | 1.688 (2) | C1—C2 | 1.390 (4) |
As1—O12 | 1.648 (2) | C1—C6 | 1.380 (4) |
As1—O13 | 1.701 (2) | C2—C3 | 1.377 (4) |
As1—C1 | 1.891 (3) | C3—C4 | 1.374 (4) |
O11—H11 | 0.88 (2) | C4—C5 | 1.386 (3) |
O13—H13 | 0.87 (3) | C5—C6 | 1.379 (4) |
N4—C4 | 1.456 (4) | C2—H2 | 0.9500 |
N4—H41 | 0.87 (2) | C3—H3 | 0.9500 |
N4—H42 | 0.87 (2) | C5—H5 | 0.9500 |
N4—H43 | 0.87 (2) | C6—H6 | 0.9500 |
O11—As1—O12 | 112.68 (11) | C2—C1—C6 | 120.9 (3) |
O11—As1—O13 | 108.54 (11) | C1—C2—C3 | 119.4 (3) |
O11—As1—C1 | 107.71 (11) | C2—C3—C4 | 119.1 (3) |
O12—As1—O13 | 111.29 (11) | N4—C4—C3 | 119.6 (2) |
O12—As1—C1 | 113.18 (11) | N4—C4—C5 | 118.2 (2) |
O13—As1—C1 | 102.89 (12) | C3—C4—C5 | 122.2 (3) |
As1—O11—H11 | 117 (2) | C4—C5—C6 | 118.4 (3) |
As1—O13—H13 | 112 (2) | C1—C6—C5 | 120.0 (3) |
H42—N4—H43 | 113 (3) | C1—C2—H2 | 120.00 |
H41—N4—H42 | 103 (2) | C3—C2—H2 | 120.00 |
H41—N4—H43 | 103 (2) | C2—C3—H3 | 120.00 |
C4—N4—H41 | 114 (2) | C4—C3—H3 | 120.00 |
C4—N4—H42 | 111.6 (18) | C4—C5—H5 | 121.00 |
C4—N4—H43 | 111.3 (15) | C6—C5—H5 | 121.00 |
As1—C1—C2 | 120.4 (2) | C1—C6—H6 | 120.00 |
As1—C1—C6 | 118.7 (2) | C5—C6—H6 | 120.00 |
O11—As1—C1—C2 | −22.9 (2) | As1—C1—C6—C5 | 178.4 (2) |
O11—As1—C1—C6 | 159.1 (2) | C2—C1—C6—C5 | 0.4 (4) |
O12—As1—C1—C2 | 102.3 (2) | C1—C2—C3—C4 | 1.2 (4) |
O12—As1—C1—C6 | −75.7 (2) | C2—C3—C4—N4 | −179.0 (3) |
O13—As1—C1—C2 | −137.5 (2) | C2—C3—C4—C5 | −0.5 (4) |
O13—As1—C1—C6 | 44.5 (2) | N4—C4—C5—C6 | 178.3 (3) |
As1—C1—C2—C3 | −179.1 (2) | C3—C4—C5—C6 | −0.3 (4) |
C6—C1—C2—C3 | −1.2 (4) | C4—C5—C6—C1 | 0.3 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O11—H11···O12i | 0.88 (2) | 1.68 (2) | 2.563 (3) | 178 (5) |
O13—H13···O12ii | 0.87 (3) | 1.73 (3) | 2.582 (3) | 167 (4) |
N4—H41···Cl1iii | 0.87 (2) | 2.29 (2) | 3.073 (2) | 151 (3) |
N4—H42···Cl1 | 0.87 (2) | 2.27 (2) | 3.091 (2) | 158 (2) |
N4—H43···Cl1iv | 0.87 (2) | 2.30 (2) | 3.160 (3) | 170 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, −y+3/2, z+1/2; (iii) x, −y−1/2, z−1/2; (iv) −x, y+1/2, −z+1/2. |
(C6H9AsNO3)2[Cu(H2O)6](SO4)2·2H2O | F(000) = 846 |
Mr = 835.92 | Dx = 1.915 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2421 reflections |
a = 15.0784 (6) Å | θ = 3.8–29.0° |
b = 11.2302 (4) Å | µ = 3.26 mm−1 |
c = 8.6756 (4) Å | T = 200 K |
β = 99.305 (4)° | Plate, colourless |
V = 1449.74 (10) Å3 | 0.30 × 0.25 × 0.08 mm |
Z = 2 |
Oxford Diffraction Gemini-S CCD-detector diffractometer | 2846 independent reflections |
Radiation source: Enhance (Mo) X-ray source | 2518 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.026 |
Detector resolution: 16.077 pixels mm-1 | θmax = 26.0°, θmin = 3.3° |
ω scans | h = −18→17 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015) | k = −13→12 |
Tmin = 0.670, Tmax = 0.980 | l = −9→10 |
6196 measured reflections |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.066 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0274P)2 + 0.3694P] where P = (Fo2 + 2Fc2)/3 |
2846 reflections | (Δ/σ)max < 0.001 |
226 parameters | Δρmax = 0.36 e Å−3 |
13 restraints | Δρmin = −0.51 e Å−3 |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles |
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 > 2sigma(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 | ||
As1 | 0.33980 (2) | 0.10571 (2) | 0.24157 (3) | 0.0172 (1) | |
O11 | 0.36399 (14) | 0.0443 (2) | 0.4232 (2) | 0.0276 (7) | |
O12 | 0.26786 (13) | 0.02573 (18) | 0.1225 (2) | 0.0249 (6) | |
O13 | 0.30451 (14) | 0.24789 (18) | 0.2623 (3) | 0.0305 (7) | |
N4 | 0.71564 (17) | 0.1526 (2) | 0.0761 (3) | 0.0174 (7) | |
C1 | 0.45558 (19) | 0.1223 (2) | 0.1863 (3) | 0.0165 (8) | |
C2 | 0.4777 (2) | 0.2222 (2) | 0.1063 (3) | 0.0205 (8) | |
C3 | 0.5634 (2) | 0.2323 (2) | 0.0701 (3) | 0.0213 (9) | |
C4 | 0.62545 (18) | 0.1425 (2) | 0.1130 (3) | 0.0158 (8) | |
C5 | 0.6026 (2) | 0.0410 (2) | 0.1881 (3) | 0.0218 (9) | |
C6 | 0.5178 (2) | 0.0313 (3) | 0.2253 (3) | 0.0222 (9) | |
Cu1 | 0.00000 | 0.00000 | 0.00000 | 0.0135 (1) | |
O1W | 0.01471 (14) | 0.10426 (18) | 0.2269 (2) | 0.0210 (6) | |
O2W | 0.10719 (14) | 0.0857 (2) | −0.0346 (2) | 0.0246 (7) | |
O3W | −0.07864 (16) | 0.13263 (18) | −0.1006 (2) | 0.0251 (7) | |
S1 | 0.83825 (5) | 0.41681 (6) | −0.01779 (7) | 0.0152 (2) | |
O1 | 0.89949 (14) | 0.33415 (17) | 0.0779 (2) | 0.0255 (7) | |
O2 | 0.85590 (14) | 0.53998 (16) | 0.0346 (2) | 0.0229 (6) | |
O3 | 0.74402 (14) | 0.38634 (16) | −0.0044 (2) | 0.0222 (6) | |
O4 | 0.84847 (14) | 0.40444 (18) | −0.1831 (2) | 0.0232 (6) | |
O4W | 0.13231 (15) | 0.30042 (17) | 0.2021 (2) | 0.0217 (7) | |
H2 | 0.43450 | 0.28290 | 0.07660 | 0.0250* | |
H3 | 0.57970 | 0.30060 | 0.01620 | 0.0260* | |
H5 | 0.64520 | −0.02130 | 0.21360 | 0.0260* | |
H6 | 0.50160 | −0.03770 | 0.27770 | 0.0270* | |
H11 | 0.3229 (18) | 0.001 (2) | 0.445 (4) | 0.0330* | |
H13 | 0.2483 (13) | 0.260 (3) | 0.246 (4) | 0.0330* | |
H41 | 0.7543 (18) | 0.137 (3) | 0.163 (3) | 0.0270* | |
H42 | 0.724 (2) | 0.2267 (18) | 0.044 (3) | 0.0270* | |
H43 | 0.720 (2) | 0.102 (2) | −0.002 (3) | 0.0270* | |
H11W | −0.0329 (16) | 0.105 (3) | 0.263 (4) | 0.0330* | |
H12W | 0.0537 (19) | 0.082 (3) | 0.296 (3) | 0.0330* | |
H21W | 0.110 (2) | 0.116 (3) | −0.123 (3) | 0.0330* | |
H22W | 0.155 (2) | 0.063 (3) | 0.018 (3) | 0.0330* | |
H31W | −0.073 (2) | 0.195 (2) | −0.050 (3) | 0.0330* | |
H32W | −0.084 (2) | 0.146 (3) | −0.197 (2) | 0.0330* | |
H41W | 0.0939 (18) | 0.249 (2) | 0.182 (4) | 0.0330* | |
H42W | 0.126 (2) | 0.343 (3) | 0.125 (3) | 0.0330* |
U11 | U22 | U33 | U12 | U13 | U23 | |
As1 | 0.0116 (2) | 0.0185 (2) | 0.0209 (2) | −0.0023 (1) | 0.0008 (1) | −0.0012 (1) |
O11 | 0.0194 (12) | 0.0386 (13) | 0.0240 (11) | −0.0124 (10) | 0.0014 (9) | 0.0042 (10) |
O12 | 0.0132 (11) | 0.0298 (11) | 0.0300 (11) | −0.0017 (9) | −0.0012 (9) | −0.0078 (9) |
O13 | 0.0149 (11) | 0.0217 (11) | 0.0546 (15) | 0.0006 (10) | 0.0050 (11) | −0.0056 (10) |
N4 | 0.0141 (13) | 0.0190 (12) | 0.0186 (12) | 0.0008 (11) | 0.0010 (10) | 0.0005 (10) |
C1 | 0.0126 (14) | 0.0174 (14) | 0.0185 (14) | −0.0032 (11) | −0.0009 (12) | −0.0011 (11) |
C2 | 0.0153 (15) | 0.0178 (14) | 0.0275 (15) | 0.0040 (12) | 0.0012 (12) | 0.0040 (12) |
C3 | 0.0205 (16) | 0.0170 (14) | 0.0259 (15) | −0.0008 (12) | 0.0021 (13) | 0.0075 (12) |
C4 | 0.0115 (14) | 0.0209 (14) | 0.0138 (13) | −0.0037 (12) | −0.0016 (11) | −0.0017 (11) |
C5 | 0.0172 (16) | 0.0189 (14) | 0.0282 (16) | 0.0049 (12) | 0.0003 (13) | 0.0061 (12) |
C6 | 0.0212 (17) | 0.0186 (14) | 0.0261 (16) | −0.0037 (12) | 0.0021 (13) | 0.0057 (12) |
Cu1 | 0.0118 (2) | 0.0143 (2) | 0.0142 (2) | 0.0003 (2) | 0.0012 (2) | 0.0011 (2) |
O1W | 0.0153 (11) | 0.0313 (12) | 0.0162 (10) | 0.0020 (10) | 0.0017 (8) | 0.0031 (9) |
O2W | 0.0157 (11) | 0.0363 (13) | 0.0212 (11) | −0.0046 (10) | 0.0013 (9) | 0.0084 (9) |
O3W | 0.0355 (14) | 0.0204 (11) | 0.0165 (10) | 0.0043 (10) | −0.0043 (10) | −0.0003 (9) |
S1 | 0.0142 (4) | 0.0175 (3) | 0.0140 (3) | −0.0002 (3) | 0.0022 (3) | −0.0002 (3) |
O1 | 0.0300 (13) | 0.0258 (11) | 0.0191 (10) | 0.0114 (10) | −0.0010 (9) | 0.0011 (9) |
O2 | 0.0261 (12) | 0.0175 (10) | 0.0227 (10) | −0.0056 (9) | −0.0028 (9) | −0.0019 (8) |
O3 | 0.0172 (11) | 0.0192 (10) | 0.0321 (12) | −0.0013 (9) | 0.0099 (9) | −0.0017 (8) |
O4 | 0.0169 (11) | 0.0391 (12) | 0.0138 (10) | −0.0023 (9) | 0.0027 (8) | −0.0027 (8) |
O4W | 0.0212 (12) | 0.0193 (11) | 0.0239 (11) | −0.0019 (9) | 0.0012 (9) | −0.0001 (9) |
Cu1—O3W | 2.013 (2) | O2W—H21W | 0.85 (3) |
Cu1—O1W | 2.2702 (18) | O3W—H31W | 0.82 (2) |
Cu1—O2W | 1.946 (2) | O3W—H32W | 0.841 (18) |
Cu1—O3Wi | 2.013 (2) | O4W—H42W | 0.82 (3) |
Cu1—O1Wi | 2.2702 (18) | O4W—H41W | 0.82 (3) |
Cu1—O2Wi | 1.946 (2) | N4—C4 | 1.451 (4) |
As1—O11 | 1.7046 (18) | N4—H42 | 0.89 (2) |
As1—O12 | 1.6395 (19) | N4—H43 | 0.90 (2) |
As1—O13 | 1.702 (2) | N4—H41 | 0.89 (3) |
As1—C1 | 1.893 (3) | C1—C2 | 1.388 (3) |
S1—O4 | 1.4736 (19) | C1—C6 | 1.392 (4) |
S1—O2 | 1.4668 (19) | C2—C3 | 1.383 (4) |
S1—O3 | 1.484 (2) | C3—C4 | 1.385 (4) |
S1—O1 | 1.468 (2) | C4—C5 | 1.384 (3) |
O11—H11 | 0.83 (3) | C5—C6 | 1.373 (4) |
O13—H13 | 0.85 (2) | C2—H2 | 0.9500 |
O1W—H12W | 0.81 (3) | C3—H3 | 0.9500 |
O1W—H11W | 0.83 (3) | C5—H5 | 0.9500 |
O2W—H22W | 0.83 (3) | C6—H6 | 0.9500 |
O11—As1—O12 | 112.44 (10) | H31W—O3W—H32W | 111 (3) |
O11—As1—O13 | 107.80 (11) | Cu1—O3W—H32W | 121 (2) |
O11—As1—C1 | 101.87 (11) | Cu1—O3W—H31W | 113.3 (19) |
O12—As1—O13 | 113.22 (11) | H41W—O4W—H42W | 105 (3) |
O12—As1—C1 | 115.95 (10) | H42—N4—H43 | 109 (2) |
O13—As1—C1 | 104.56 (10) | H41—N4—H42 | 110 (3) |
O2W—Cu1—O3W | 90.74 (9) | H41—N4—H43 | 113 (3) |
O1Wi—Cu1—O2W | 95.08 (8) | C4—N4—H41 | 107.8 (17) |
O2W—Cu1—O2Wi | 180.00 | C4—N4—H42 | 109.0 (19) |
O2W—Cu1—O3Wi | 89.26 (9) | C4—N4—H43 | 107.7 (19) |
O1Wi—Cu1—O3W | 92.15 (7) | As1—C1—C2 | 120.8 (2) |
O3W—Cu1—O3Wi | 180.00 | As1—C1—C6 | 118.6 (2) |
O1W—Cu1—O1Wi | 180.00 | C2—C1—C6 | 120.5 (3) |
O1W—Cu1—O2W | 84.92 (8) | C1—C2—C3 | 119.3 (2) |
O1W—Cu1—O3W | 87.85 (7) | C2—C3—C4 | 119.7 (2) |
O3—S1—O4 | 107.85 (11) | N4—C4—C3 | 120.0 (2) |
O2—S1—O4 | 110.38 (11) | N4—C4—C5 | 118.8 (2) |
O1—S1—O3 | 109.42 (11) | C3—C4—C5 | 121.2 (3) |
O1—S1—O4 | 109.60 (12) | C4—C5—C6 | 119.2 (3) |
O1—S1—O2 | 110.79 (11) | C1—C6—C5 | 120.1 (3) |
O2—S1—O3 | 108.74 (12) | C1—C2—H2 | 120.00 |
As1—O11—H11 | 113 (2) | C3—C2—H2 | 120.00 |
As1—O13—H13 | 117 (2) | C2—C3—H3 | 120.00 |
H11W—O1W—H12W | 107 (3) | C4—C3—H3 | 120.00 |
Cu1—O1W—H12W | 116 (2) | C4—C5—H5 | 120.00 |
Cu1—O1W—H11W | 111 (2) | C6—C5—H5 | 120.00 |
H21W—O2W—H22W | 117 (3) | C1—C6—H6 | 120.00 |
Cu1—O2W—H22W | 116 (2) | C5—C6—H6 | 120.00 |
Cu1—O2W—H21W | 120 (2) | ||
O11—As1—C1—C2 | −140.8 (2) | As1—C1—C6—C5 | −179.4 (2) |
O11—As1—C1—C6 | 40.3 (2) | C2—C1—C6—C5 | 1.6 (4) |
O12—As1—C1—C2 | 96.8 (2) | C1—C2—C3—C4 | 0.5 (4) |
O12—As1—C1—C6 | −82.2 (2) | C2—C3—C4—N4 | −179.7 (2) |
O13—As1—C1—C2 | −28.6 (2) | C2—C3—C4—C5 | 1.7 (4) |
O13—As1—C1—C6 | 152.4 (2) | N4—C4—C5—C6 | 179.2 (2) |
As1—C1—C2—C3 | 178.93 (19) | C3—C4—C5—C6 | −2.3 (4) |
C6—C1—C2—C3 | −2.1 (4) | C4—C5—C6—C1 | 0.6 (4) |
Symmetry code: (i) −x, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O11—H11···O3ii | 0.83 (3) | 1.76 (3) | 2.582 (3) | 167 (3) |
O13—H13···O4W | 0.85 (2) | 1.79 (2) | 2.631 (3) | 174 (3) |
O1W—H11W···O4iii | 0.83 (3) | 1.92 (3) | 2.745 (3) | 171 (4) |
O1W—H12W···O2ii | 0.81 (3) | 1.90 (3) | 2.703 (3) | 176 (3) |
O2W—H21W···O4Wiv | 0.85 (3) | 1.86 (3) | 2.698 (3) | 170 (3) |
O2W—H22W···O12 | 0.83 (3) | 1.84 (3) | 2.667 (3) | 173 (3) |
O3W—H31W···O1v | 0.82 (2) | 2.00 (2) | 2.792 (3) | 161 (3) |
O3W—H32W···O1vi | 0.84 (2) | 1.94 (2) | 2.780 (2) | 176 (4) |
O4W—H41W···O1W | 0.82 (3) | 2.09 (3) | 2.858 (3) | 157 (3) |
O4W—H42W···O2vii | 0.82 (3) | 1.96 (3) | 2.753 (3) | 164 (3) |
N4—H41···O4viii | 0.89 (3) | 1.85 (3) | 2.726 (3) | 169 (3) |
N4—H42···O3 | 0.89 (2) | 1.88 (2) | 2.767 (3) | 175 (2) |
N4—H43···O12ix | 0.90 (2) | 1.80 (2) | 2.680 (3) | 166 (2) |
C2—H2···O11iv | 0.95 | 2.49 | 3.385 (3) | 157 |
Symmetry codes: (ii) −x+1, y−1/2, −z+1/2; (iii) x−1, −y+1/2, z+1/2; (iv) x, −y+1/2, z−1/2; (v) x−1, y, z; (vi) x−1, −y+1/2, z−1/2; (vii) −x+1, −y+1, −z; (viii) x, −y+1/2, z+1/2; (ix) −x+1, −y, −z. |
(C6H9AsNO3)2[CuCl4] | F(000) = 1260 |
Mr = 641.47 | Dx = 2.057 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 1633 reflections |
a = 7.6315 (4) Å | θ = 3.9–29.0° |
b = 7.1244 (4) Å | µ = 4.77 mm−1 |
c = 38.0925 (15) Å | T = 200 K |
V = 2071.08 (18) Å3 | Plate, green |
Z = 4 | 0.25 × 0.25 × 0.04 mm |
Oxford Diffraction Gemini-S CCD-detector diffractometer | 2028 independent reflections |
Radiation source: Enhance (Mo) X-ray source | 1715 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
Detector resolution: 16.077 pixels mm-1 | θmax = 26.0°, θmin = 3.2° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015) | k = −3→8 |
Tmin = 0.544, Tmax = 0.980 | l = −46→28 |
6065 measured reflections |
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) = 0.090 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0415P)2 + 0.2932P] where P = (Fo2 + 2Fc2)/3 |
2028 reflections | (Δ/σ)max = 0.001 |
139 parameters | Δρmax = 0.42 e Å−3 |
5 restraints | Δρmin = −0.57 e Å−3 |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles |
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 > 2sigma(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 | ||
Cu1 | 0.50000 | 0.50000 | 0.50000 | 0.0224 (2) | |
Cl1 | 0.54832 (12) | 0.52358 (15) | 0.44103 (2) | 0.0294 (3) | |
Cl2 | 0.70111 (12) | 0.73489 (12) | 0.50945 (3) | 0.0288 (3) | |
As1 | 1.05548 (5) | 0.75093 (6) | 0.29143 (1) | 0.0228 (1) | |
O11 | 1.2663 (3) | 0.8193 (4) | 0.28480 (7) | 0.0352 (9) | |
O12 | 0.9644 (3) | 0.6341 (4) | 0.25899 (6) | 0.0336 (9) | |
O13 | 0.9462 (4) | 0.9566 (4) | 0.29820 (8) | 0.0363 (10) | |
N4 | 0.9665 (5) | 0.4774 (5) | 0.44152 (9) | 0.0291 (11) | |
C1 | 1.0413 (4) | 0.6402 (6) | 0.33687 (9) | 0.0226 (11) | |
C2 | 1.1575 (5) | 0.6990 (6) | 0.36228 (9) | 0.0318 (14) | |
C3 | 1.1353 (5) | 0.6432 (6) | 0.39646 (9) | 0.0296 (11) | |
C4 | 0.9985 (5) | 0.5270 (5) | 0.40483 (10) | 0.0244 (11) | |
C5 | 0.8857 (5) | 0.4604 (6) | 0.37931 (10) | 0.0360 (13) | |
C6 | 0.9080 (5) | 0.5174 (6) | 0.34507 (10) | 0.0334 (13) | |
H2 | 1.25290 | 0.77810 | 0.35610 | 0.0380* | |
H3 | 1.21400 | 0.68470 | 0.41410 | 0.0360* | |
H5 | 0.79390 | 0.37630 | 0.38530 | 0.0430* | |
H6 | 0.83200 | 0.47230 | 0.32720 | 0.0400* | |
H11 | 1.321 (5) | 0.750 (5) | 0.2708 (11) | 0.0530* | |
H13 | 0.961 (6) | 1.033 (6) | 0.2812 (10) | 0.0550* | |
H41 | 0.985 (5) | 0.356 (3) | 0.4438 (11) | 0.0350* | |
H42 | 1.046 (4) | 0.530 (6) | 0.4545 (10) | 0.0350* | |
H43 | 0.859 (3) | 0.506 (5) | 0.4486 (10) | 0.0350* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cu1 | 0.0255 (3) | 0.0225 (4) | 0.0191 (3) | −0.0066 (3) | 0.0005 (3) | 0.0006 (3) |
Cl1 | 0.0326 (5) | 0.0355 (6) | 0.0200 (5) | −0.0028 (4) | 0.0018 (4) | 0.0006 (4) |
Cl2 | 0.0300 (5) | 0.0261 (5) | 0.0302 (5) | −0.0094 (4) | −0.0015 (4) | −0.0001 (4) |
As1 | 0.0241 (2) | 0.0295 (3) | 0.0149 (2) | 0.0019 (2) | 0.0007 (1) | 0.0009 (2) |
O11 | 0.0292 (15) | 0.0446 (19) | 0.0319 (15) | −0.0032 (14) | 0.0086 (12) | −0.0056 (14) |
O12 | 0.0379 (15) | 0.0431 (19) | 0.0198 (14) | −0.0001 (13) | −0.0064 (11) | −0.0016 (13) |
O13 | 0.0402 (16) | 0.0367 (19) | 0.0321 (15) | 0.0121 (13) | 0.0116 (13) | 0.0076 (14) |
N4 | 0.0339 (18) | 0.033 (2) | 0.0204 (17) | 0.0044 (16) | 0.0026 (14) | 0.0052 (16) |
C1 | 0.0260 (18) | 0.024 (2) | 0.0177 (18) | 0.0011 (15) | −0.0012 (14) | 0.0035 (16) |
C2 | 0.033 (2) | 0.039 (3) | 0.0234 (19) | −0.0129 (18) | −0.0010 (16) | 0.0047 (18) |
C3 | 0.033 (2) | 0.034 (2) | 0.0219 (18) | −0.0086 (18) | −0.0082 (16) | −0.0007 (18) |
C4 | 0.0273 (19) | 0.025 (2) | 0.0208 (19) | 0.0033 (16) | 0.0045 (15) | 0.0024 (16) |
C5 | 0.036 (2) | 0.048 (3) | 0.0240 (18) | −0.020 (2) | −0.0017 (18) | 0.0030 (19) |
C6 | 0.032 (2) | 0.047 (3) | 0.0212 (18) | −0.0145 (19) | −0.0070 (17) | −0.0005 (19) |
Cu1—Cl2i | 2.2990 (9) | N4—H41 | 0.88 (2) |
Cu1—Cl2ii | 2.9833 (9) | N4—H42 | 0.87 (4) |
Cu1—Cl1i | 2.2826 (8) | N4—H43 | 0.89 (3) |
Cu1—Cl1 | 2.2826 (8) | C1—C2 | 1.378 (5) |
Cu1—Cl2 | 2.2990 (9) | C1—C6 | 1.378 (5) |
Cu1—Cl2iii | 2.9833 (9) | C2—C3 | 1.372 (5) |
As1—O12 | 1.644 (2) | C3—C4 | 1.370 (5) |
As1—O13 | 1.706 (3) | C4—C5 | 1.383 (5) |
As1—C1 | 1.905 (4) | C5—C6 | 1.377 (5) |
As1—O11 | 1.700 (2) | C2—H2 | 0.9500 |
O11—H11 | 0.84 (4) | C3—H3 | 0.9500 |
O13—H13 | 0.85 (4) | C5—H5 | 0.9500 |
N4—C4 | 1.462 (5) | C6—H6 | 0.9500 |
O11—As1—C1 | 107.90 (13) | C4—N4—H42 | 109 (2) |
O11—As1—O12 | 115.70 (12) | C4—N4—H43 | 113 (2) |
O11—As1—O13 | 103.83 (14) | As1—C1—C2 | 118.4 (3) |
O13—As1—C1 | 100.98 (16) | As1—C1—C6 | 120.7 (3) |
O12—As1—O13 | 109.99 (14) | C2—C1—C6 | 120.6 (3) |
O12—As1—C1 | 116.69 (15) | C1—C2—C3 | 119.9 (4) |
Cl1—Cu1—Cl2 | 89.58 (4) | C2—C3—C4 | 119.4 (4) |
Cl2—Cu1—Cl2i | 180.00 | N4—C4—C3 | 119.7 (3) |
Cl2—Cu1—Cl2ii | 86.07 (3) | N4—C4—C5 | 119.0 (3) |
Cl1i—Cu1—Cl2iii | 92.40 (3) | C3—C4—C5 | 121.2 (4) |
Cl2i—Cu1—Cl2ii | 93.93 (3) | C4—C5—C6 | 119.2 (4) |
Cl1—Cu1—Cl2i | 90.42 (4) | C1—C6—C5 | 119.6 (4) |
Cl1—Cu1—Cl2iii | 87.60 (3) | C1—C2—H2 | 120.00 |
Cl1—Cu1—Cl1i | 180.00 | C3—C2—H2 | 120.00 |
Cu1—Cl2—Cu1iv | 162.25 (5) | C2—C3—H3 | 120.00 |
As1—O11—H11 | 113 (3) | C4—C3—H3 | 120.00 |
As1—O13—H13 | 112 (3) | C4—C5—H5 | 120.00 |
H42—N4—H43 | 112 (3) | C6—C5—H5 | 120.00 |
H41—N4—H42 | 105 (4) | C1—C6—H6 | 120.00 |
H41—N4—H43 | 110 (3) | C5—C6—H6 | 120.00 |
C4—N4—H41 | 108 (3) | ||
O11—As1—C1—C2 | 28.1 (4) | As1—C1—C6—C5 | −170.7 (3) |
O11—As1—C1—C6 | −157.8 (3) | C2—C1—C6—C5 | 3.2 (6) |
O12—As1—C1—C2 | 160.4 (3) | C1—C2—C3—C4 | 0.9 (6) |
O12—As1—C1—C6 | −25.6 (4) | C2—C3—C4—N4 | −175.7 (4) |
O13—As1—C1—C2 | −80.4 (3) | C2—C3—C4—C5 | 2.0 (6) |
O13—As1—C1—C6 | 93.6 (3) | N4—C4—C5—C6 | 175.5 (4) |
As1—C1—C2—C3 | 170.5 (3) | C3—C4—C5—C6 | −2.3 (6) |
C6—C1—C2—C3 | −3.5 (6) | C4—C5—C6—C1 | −0.3 (6) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+3/2, y−1/2, z; (iii) x−1/2, −y+3/2, −z+1; (iv) x+1/2, −y+3/2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O11—H11···O12v | 0.84 (4) | 1.78 (4) | 2.609 (4) | 170 (3) |
O13—H13···O12vi | 0.85 (4) | 1.79 (4) | 2.610 (4) | 162 (4) |
N4—H41···Cl1ii | 0.88 (2) | 2.38 (2) | 3.235 (4) | 163 (4) |
N4—H42···Cl2iv | 0.87 (4) | 2.47 (4) | 3.301 (4) | 161 (3) |
N4—H43···Cl1 | 0.89 (3) | 2.39 (2) | 3.208 (4) | 153 (3) |
C6—H6···O13ii | 0.95 | 2.40 | 3.268 (5) | 152 |
Symmetry codes: (ii) −x+3/2, y−1/2, z; (iv) x+1/2, −y+3/2, −z+1; (v) x+1/2, y, −z+1/2; (vi) −x+2, y+1/2, −z+1/2. |
(C6H9AsNO3)2[CdCl4] | F(000) = 1336 |
Mr = 690.32 | Dx = 2.168 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 1959 reflections |
a = 7.5525 (4) Å | θ = 3.9–28.7° |
b = 7.2578 (3) Å | µ = 4.67 mm−1 |
c = 38.5872 (17) Å | T = 200 K |
V = 2115.14 (17) Å3 | Plate, colourless |
Z = 4 | 0.41 × 0.25 × 0.10 mm |
Oxford Diffraction Gemini-S CCD-detector diffractometer | 2070 independent reflections |
Radiation source: ENHANCE (Mo) X-ray source | 1778 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 16.077 pixels mm-1 | θmax = 26.0°, θmin = 3.4° |
ω scans | h = −9→6 |
Absorption correction: multi-scan (CrysAlis PRO; Rigaku OD, 2015 | k = −8→7 |
Tmin = 0.485, Tmax = 0.980 | l = −44→47 |
5452 measured reflections |
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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.070 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0265P)2] where P = (Fo2 + 2Fc2)/3 |
2070 reflections | (Δ/σ)max = 0.001 |
139 parameters | Δρmax = 0.62 e Å−3 |
5 restraints | Δρmin = −0.50 e Å−3 |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles |
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 > 2sigma(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 | ||
Cd1 | 0.50000 | 0.50000 | 0.50000 | 0.0145 (1) | |
Cl1 | 0.55662 (14) | 0.52125 (14) | 0.43568 (3) | 0.0211 (3) | |
Cl2 | 0.70634 (14) | 0.79615 (13) | 0.50986 (3) | 0.0194 (3) | |
As1 | 1.05703 (6) | 0.75535 (6) | 0.29043 (1) | 0.0155 (1) | |
O11 | 1.2690 (4) | 0.8254 (4) | 0.28422 (7) | 0.0237 (10) | |
O12 | 0.9688 (4) | 0.6397 (4) | 0.25798 (7) | 0.0222 (9) | |
O13 | 0.9450 (4) | 0.9568 (4) | 0.29732 (8) | 0.0251 (10) | |
N4 | 0.9693 (5) | 0.4583 (5) | 0.43687 (9) | 0.0203 (11) | |
C1 | 1.0425 (6) | 0.6420 (6) | 0.33478 (9) | 0.0161 (11) | |
C2 | 1.1509 (6) | 0.7069 (6) | 0.36094 (10) | 0.0227 (14) | |
C3 | 1.1299 (6) | 0.6438 (6) | 0.39430 (10) | 0.0213 (12) | |
C4 | 1.0021 (5) | 0.5170 (5) | 0.40065 (10) | 0.0160 (12) | |
C5 | 0.8963 (6) | 0.4450 (6) | 0.37506 (11) | 0.0253 (16) | |
C6 | 0.9169 (6) | 0.5087 (6) | 0.34161 (10) | 0.0233 (14) | |
H2 | 1.24010 | 0.79520 | 0.35590 | 0.0270* | |
H3 | 1.20330 | 0.68800 | 0.41250 | 0.0260* | |
H5 | 0.81070 | 0.35320 | 0.38030 | 0.0310* | |
H6 | 0.84530 | 0.46130 | 0.32340 | 0.0280* | |
H11 | 1.331 (6) | 0.758 (5) | 0.2703 (10) | 0.0360* | |
H13 | 0.952 (6) | 1.034 (5) | 0.2798 (9) | 0.0380* | |
H41 | 0.974 (6) | 0.337 (3) | 0.4383 (12) | 0.0240* | |
H42 | 1.048 (5) | 0.515 (5) | 0.4508 (10) | 0.0240* | |
H43 | 0.858 (3) | 0.492 (5) | 0.4422 (11) | 0.0240* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0138 (2) | 0.0150 (2) | 0.0146 (2) | −0.0006 (2) | 0.0006 (2) | 0.0013 (2) |
Cl1 | 0.0220 (6) | 0.0257 (6) | 0.0155 (5) | 0.0001 (4) | 0.0018 (4) | −0.0001 (4) |
Cl2 | 0.0191 (5) | 0.0182 (5) | 0.0210 (5) | −0.0071 (4) | 0.0016 (4) | −0.0006 (4) |
As1 | 0.0148 (2) | 0.0205 (2) | 0.0112 (2) | 0.0011 (2) | 0.0003 (2) | 0.0006 (2) |
O11 | 0.0169 (17) | 0.0326 (18) | 0.0215 (15) | −0.0013 (14) | 0.0061 (13) | −0.0052 (14) |
O12 | 0.0217 (17) | 0.0261 (16) | 0.0187 (15) | 0.0003 (14) | −0.0056 (13) | −0.0027 (13) |
O13 | 0.0287 (19) | 0.0232 (17) | 0.0233 (16) | 0.0094 (14) | 0.0066 (15) | 0.0043 (13) |
N4 | 0.019 (2) | 0.027 (2) | 0.0149 (18) | 0.0003 (17) | 0.0016 (16) | 0.0017 (16) |
C1 | 0.020 (2) | 0.017 (2) | 0.0113 (19) | 0.0024 (18) | −0.0014 (17) | 0.0020 (16) |
C2 | 0.024 (3) | 0.027 (2) | 0.017 (2) | −0.011 (2) | −0.0014 (19) | 0.0017 (18) |
C3 | 0.025 (2) | 0.025 (2) | 0.014 (2) | −0.006 (2) | −0.0034 (18) | 0.0014 (18) |
C4 | 0.016 (2) | 0.015 (2) | 0.017 (2) | 0.0051 (17) | 0.0032 (18) | −0.0002 (16) |
C5 | 0.021 (3) | 0.033 (3) | 0.022 (2) | −0.014 (2) | 0.001 (2) | 0.002 (2) |
C6 | 0.021 (2) | 0.034 (3) | 0.015 (2) | −0.007 (2) | −0.0064 (19) | −0.0040 (19) |
Cd1—Cl2i | 2.6820 (10) | N4—H41 | 0.88 (2) |
Cd1—Cl2ii | 2.6931 (10) | N4—H42 | 0.90 (4) |
Cd1—Cl1i | 2.5232 (12) | N4—H43 | 0.90 (3) |
Cd1—Cl1 | 2.5232 (12) | C1—C2 | 1.382 (6) |
Cd1—Cl2 | 2.6820 (10) | C1—C6 | 1.380 (6) |
Cd1—Cl2iii | 2.6931 (10) | C2—C3 | 1.376 (6) |
As1—O11 | 1.697 (3) | C3—C4 | 1.356 (6) |
As1—O12 | 1.648 (3) | C4—C5 | 1.374 (6) |
As1—O13 | 1.710 (3) | C5—C6 | 1.380 (6) |
As1—C1 | 1.902 (4) | C2—H2 | 0.9500 |
O11—H11 | 0.86 (4) | C3—H3 | 0.9500 |
O13—H13 | 0.88 (4) | C5—H5 | 0.9500 |
N4—C4 | 1.482 (5) | C6—H6 | 0.9500 |
Cl1—Cd1—Cl2 | 89.55 (3) | C4—N4—H41 | 110 (3) |
Cl1—Cd1—Cl2iii | 88.11 (3) | C4—N4—H42 | 109 (2) |
Cl1—Cd1—Cl1i | 180.00 | C4—N4—H43 | 107 (3) |
Cl1—Cd1—Cl2i | 90.45 (3) | As1—C1—C2 | 118.4 (3) |
Cl1—Cd1—Cl2ii | 91.89 (3) | As1—C1—C6 | 121.0 (3) |
Cl2—Cd1—Cl2iii | 93.34 (3) | C2—C1—C6 | 120.4 (4) |
Cl1i—Cd1—Cl2 | 90.45 (3) | C1—C2—C3 | 120.1 (4) |
Cl2—Cd1—Cl2i | 180.00 | C2—C3—C4 | 118.5 (4) |
Cl2—Cd1—Cl2ii | 86.66 (3) | N4—C4—C3 | 119.0 (3) |
O11—As1—C1 | 108.13 (17) | N4—C4—C5 | 118.1 (3) |
O11—As1—O12 | 115.27 (14) | C3—C4—C5 | 122.9 (4) |
O11—As1—O13 | 103.45 (14) | C4—C5—C6 | 118.7 (4) |
O13—As1—C1 | 101.62 (17) | C1—C6—C5 | 119.4 (4) |
O12—As1—O13 | 110.70 (15) | C1—C2—H2 | 120.00 |
O12—As1—C1 | 116.10 (16) | C3—C2—H2 | 120.00 |
Cd1—Cl2—Cd1iv | 154.00 (4) | C2—C3—H3 | 121.00 |
As1—O11—H11 | 115 (3) | C4—C3—H3 | 121.00 |
As1—O13—H13 | 113 (3) | C4—C5—H5 | 121.00 |
H42—N4—H43 | 111 (3) | C6—C5—H5 | 121.00 |
H41—N4—H42 | 113 (4) | C1—C6—H6 | 120.00 |
H41—N4—H43 | 107 (4) | C5—C6—H6 | 120.00 |
Cl1—Cd1—Cl2—Cd1iv | −45.92 (10) | As1—C1—C6—C5 | −172.4 (3) |
O11—As1—C1—C2 | 32.4 (4) | C2—C1—C6—C5 | 2.2 (7) |
O11—As1—C1—C6 | −152.9 (3) | C1—C2—C3—C4 | 0.4 (7) |
O12—As1—C1—C2 | 163.8 (3) | C2—C3—C4—N4 | −175.5 (4) |
O12—As1—C1—C6 | −21.6 (4) | C2—C3—C4—C5 | 2.0 (6) |
O13—As1—C1—C2 | −76.1 (4) | N4—C4—C5—C6 | 175.3 (4) |
O13—As1—C1—C6 | 98.6 (4) | C3—C4—C5—C6 | −2.2 (6) |
As1—C1—C2—C3 | 172.3 (3) | C4—C5—C6—C1 | 0.1 (6) |
C6—C1—C2—C3 | −2.4 (7) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+3/2, y−1/2, z; (iii) x−1/2, −y+3/2, −z+1; (iv) x+1/2, −y+3/2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O11—H11···O12v | 0.86 (4) | 1.74 (4) | 2.597 (4) | 175 (3) |
O13—H13···O12vi | 0.88 (4) | 1.75 (4) | 2.596 (4) | 160 (4) |
N4—H41···Cl1ii | 0.88 (2) | 2.31 (2) | 3.178 (4) | 170 (5) |
N4—H42···Cl2iv | 0.90 (4) | 2.37 (4) | 3.257 (4) | 168 (3) |
N4—H43···Cl1 | 0.90 (3) | 2.30 (2) | 3.150 (4) | 158 (4) |
C6—H6···O13ii | 0.95 | 2.41 | 3.246 (5) | 146 |
Symmetry codes: (ii) −x+3/2, y−1/2, z; (iv) x+1/2, −y+3/2, −z+1; (v) x+1/2, y, −z+1/2; (vi) −x+2, y+1/2, −z+1/2. |