Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803026242/su6056sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803026242/su6056Isup2.hkl |
CCDC reference: 227757
Key indicators
- Single-crystal X-ray study
- T = 120 K
- Mean (C-C) = 0.006 Å
- R factor = 0.045
- wR factor = 0.112
- Data-to-parameter ratio = 24.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ..... = 5
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.122 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.99 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.02 PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 13 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.72 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.09 Ratio PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor .... 2.40 PLAT301_ALERT_3_C Main Residue Disorder ......................... 21.00 Perc. PLAT757_ALERT_4_C D...A Calc 2.82305, Rep 2.823(3) ...... Senseless su N2 -O5 1.555 1.555 PLAT757_ALERT_4_C D...A Calc 2.73141, Rep 2.731(3) ...... Senseless su O5 -O3 1.555 1.455 PLAT757_ALERT_4_C D...A Calc 2.82515, Rep 2.825(2) ...... Senseless su O5 -O2 1.555 2.656 PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.12 Ratio PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.40 Deg. C9B -C8 -C9A 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 15 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 6 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: COLLECT (Enraf-Nonius, 1999); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and ATOMS (Shape software, 1999); software used to prepare material for publication: SHELXL97.
(C7H10N)2[HAsO4]·H2O | Z = 2 |
Mr = 374.26 | F(000) = 388 |
Triclinic, P1 | Dx = 1.483 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.4400 (2) Å | Cell parameters from 24435 reflections |
b = 8.9128 (3) Å | θ = 2.9–27.5° |
c = 14.9957 (5) Å | µ = 2.05 mm−1 |
α = 99.7048 (11)° | T = 120 K |
β = 93.1574 (12)° | Plate, colourless |
γ = 97.7776 (18)° | 0.35 × 0.12 × 0.03 mm |
V = 837.93 (5) Å3 |
Enraf-Nonius KappaCCD diffractometer | 3846 independent reflections |
Radiation source: fine-focus sealed tube | 3538 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.122 |
ω and φ scans | θmax = 27.5°, θmin = 2.9° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995) | h = −8→8 |
Tmin = 0.534, Tmax = 0.941 | k = −11→11 |
18359 measured reflections | l = −19→19 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.045 | H-atom parameters constrained |
wR(F2) = 0.112 | w = 1/[σ2(Fo2) + (0.0281P)2 + 2.1999P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
3846 reflections | Δρmax = 1.39 e Å−3 |
158 parameters | Δρmin = −0.69 e Å−3 |
0 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.021 (2) |
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 | Occ. (<1) | |
As1 | 0.79069 (5) | 0.27362 (3) | 0.455577 (19) | 0.01615 (13) | |
O1 | 0.5423 (3) | 0.3057 (2) | 0.44548 (14) | 0.0206 (4) | |
O2 | 0.8133 (3) | 0.0866 (2) | 0.43007 (14) | 0.0199 (4) | |
O3 | 0.9006 (3) | 0.3503 (2) | 0.56046 (14) | 0.0198 (4) | |
O4 | 0.9323 (4) | 0.3618 (3) | 0.37887 (14) | 0.0242 (5) | |
H1 | 0.9963 | 0.4563 | 0.4027 | 0.029* | |
N1 | 0.2439 (4) | 0.0543 (3) | 0.41567 (17) | 0.0191 (5) | |
H4 | 0.2482 | 0.0079 | 0.4652 | 0.023* | |
H5 | 0.1122 | 0.0767 | 0.4048 | 0.023* | |
H6 | 0.3375 | 0.1428 | 0.4261 | 0.023* | |
C1 | 0.3001 (5) | −0.0517 (4) | 0.3348 (2) | 0.0219 (6) | |
H10 | 0.2091 | −0.1524 | 0.3282 | 0.026* | |
H11 | 0.4477 | −0.0687 | 0.3447 | 0.026* | |
C2 | 0.2742 (5) | 0.0126 (3) | 0.2489 (2) | 0.0225 (6) | |
C3 | 0.4443 (7) | 0.0443 (5) | 0.1989 (3) | 0.0355 (8) | |
H12 | 0.5806 | 0.0292 | 0.2198 | 0.043* | |
C4 | 0.4147 (8) | 0.0988 (5) | 0.1177 (3) | 0.0438 (10) | |
H13 | 0.5314 | 0.1191 | 0.0832 | 0.053* | |
C5 | 0.2200 (8) | 0.1232 (5) | 0.0871 (2) | 0.0421 (10) | |
H14 | 0.2015 | 0.1603 | 0.0319 | 0.050* | |
C6 | 0.0526 (8) | 0.0937 (6) | 0.1370 (3) | 0.0593 (15) | |
H15 | −0.0827 | 0.1114 | 0.1164 | 0.071* | |
C7 | 0.0783 (7) | 0.0382 (6) | 0.2174 (3) | 0.0470 (11) | |
H16 | −0.0397 | 0.0175 | 0.2511 | 0.056* | |
N2 | 0.5536 (4) | 0.4647 (3) | 0.64221 (17) | 0.0208 (5) | |
H7 | 0.5098 | 0.5232 | 0.6027 | 0.025* | |
H8 | 0.4500 | 0.3855 | 0.6446 | 0.025* | |
H9 | 0.6708 | 0.4266 | 0.6232 | 0.025* | |
C8 | 0.6026 (2) | 0.56092 (16) | 0.73401 (9) | 0.0285 (7) | |
H17 | 0.4768 | 0.6071 | 0.7527 | 0.034* | |
H18 | 0.7167 | 0.6460 | 0.7312 | 0.034* | |
C9A | 0.6777 (2) | 0.47374 (16) | 0.80588 (9) | 0.023 (3)* | 0.50 |
C10A | 0.8731 (2) | 0.42391 (16) | 0.80400 (9) | 0.0350 (15)* | 0.596 (7) |
H10A | 0.9619 | 0.4441 | 0.7575 | 0.042* | 0.596 (7) |
C11A | 0.9386 (2) | 0.34449 (16) | 0.87007 (9) | 0.0428 (17)* | 0.596 (7) |
H11A | 1.0722 | 0.3104 | 0.8688 | 0.051* | 0.596 (7) |
C12A | 0.8088 (2) | 0.31491 (16) | 0.93803 (9) | 0.049 (2)* | 0.596 (7) |
H12A | 0.8536 | 0.2606 | 0.9832 | 0.059* | 0.596 (7) |
C13A | 0.6134 (2) | 0.36474 (16) | 0.93991 (9) | 0.0471 (19)* | 0.596 (7) |
H13A | 0.5247 | 0.3445 | 0.9864 | 0.057* | 0.596 (7) |
C14A | 0.5479 (2) | 0.44416 (16) | 0.87384 (9) | 0.0403 (17)* | 0.596 (7) |
H14A | 0.4144 | 0.4782 | 0.8751 | 0.048* | 0.596 (7) |
C9B | 0.6550 (2) | 0.46838 (16) | 0.80328 (9) | 0.028 (3)* | 0.50 |
C10B | 0.8649 (2) | 0.47486 (16) | 0.83297 (9) | 0.034 (2)* | 0.404 (7) |
H10B | 0.9716 | 0.5340 | 0.8070 | 0.041* | 0.404 (7) |
C11B | 0.9186 (2) | 0.39476 (16) | 0.90066 (9) | 0.033 (2)* | 0.404 (7) |
H11B | 1.0621 | 0.3992 | 0.9210 | 0.040* | 0.404 (7) |
C12B | 0.7625 (2) | 0.30818 (16) | 0.93865 (9) | 0.027 (2)* | 0.404 (7) |
H12B | 0.7993 | 0.2534 | 0.9849 | 0.033* | 0.404 (7) |
C13B | 0.5527 (2) | 0.30170 (16) | 0.90895 (9) | 0.030 (2)* | 0.404 (7) |
H13B | 0.4460 | 0.2425 | 0.9349 | 0.036* | 0.404 (7) |
C14B | 0.4989 (2) | 0.38179 (16) | 0.84127 (9) | 0.0250 (19)* | 0.404 (7) |
H14B | 0.3555 | 0.3774 | 0.8210 | 0.030* | 0.404 (7) |
O5 | 0.2125 (2) | 0.22976 (16) | 0.64252 (9) | 0.0247 (5) | |
H2 | 0.0966 | 0.2619 | 0.6114 | 0.030* | |
H3 | 0.2019 | 0.1337 | 0.6227 | 0.030* |
U11 | U22 | U33 | U12 | U13 | U23 | |
As1 | 0.02293 (19) | 0.00932 (18) | 0.01604 (18) | 0.00171 (11) | 0.00122 (11) | 0.00244 (11) |
O1 | 0.0236 (11) | 0.0138 (10) | 0.0238 (11) | 0.0024 (8) | −0.0011 (9) | 0.0032 (8) |
O2 | 0.0276 (11) | 0.0085 (9) | 0.0233 (11) | 0.0041 (8) | 0.0021 (9) | 0.0007 (8) |
O3 | 0.0272 (11) | 0.0123 (10) | 0.0182 (10) | −0.0002 (8) | −0.0023 (8) | 0.0012 (8) |
O4 | 0.0338 (13) | 0.0158 (10) | 0.0201 (11) | −0.0056 (9) | 0.0068 (9) | 0.0006 (8) |
N1 | 0.0233 (13) | 0.0141 (12) | 0.0201 (12) | 0.0010 (10) | 0.0003 (10) | 0.0057 (10) |
C1 | 0.0302 (16) | 0.0152 (14) | 0.0207 (15) | 0.0041 (12) | 0.0037 (12) | 0.0034 (11) |
C2 | 0.0322 (17) | 0.0156 (14) | 0.0175 (14) | −0.0014 (12) | 0.0008 (12) | 0.0012 (11) |
C3 | 0.047 (2) | 0.035 (2) | 0.0308 (18) | 0.0178 (17) | 0.0169 (16) | 0.0113 (15) |
C4 | 0.069 (3) | 0.038 (2) | 0.032 (2) | 0.016 (2) | 0.026 (2) | 0.0133 (17) |
C5 | 0.071 (3) | 0.030 (2) | 0.0209 (17) | −0.0076 (19) | −0.0081 (18) | 0.0076 (14) |
C6 | 0.048 (3) | 0.077 (4) | 0.054 (3) | −0.019 (2) | −0.024 (2) | 0.044 (3) |
C7 | 0.032 (2) | 0.066 (3) | 0.045 (2) | −0.0119 (19) | −0.0092 (17) | 0.037 (2) |
N2 | 0.0300 (14) | 0.0135 (12) | 0.0196 (12) | 0.0052 (10) | 0.0020 (10) | 0.0031 (10) |
C8 | 0.051 (2) | 0.0137 (15) | 0.0203 (15) | 0.0066 (14) | 0.0046 (14) | −0.0011 (12) |
O5 | 0.0300 (12) | 0.0138 (10) | 0.0292 (12) | 0.0031 (9) | −0.0025 (9) | 0.0022 (9) |
As1—O1 | 1.666 (2) | C8—C9A | 1.5252 |
As1—O2 | 1.675 (2) | C8—H17 | 0.9900 |
As1—O3 | 1.681 (2) | C8—H18 | 0.9900 |
As1—O4 | 1.732 (2) | C9A—C10A | 1.3900 |
O4—H1 | 0.8919 | C9A—C14A | 1.3900 |
N1—C1 | 1.499 (4) | C10A—C11A | 1.3900 |
N1—H4 | 0.9100 | C10A—H10A | 0.9500 |
N1—H5 | 0.9100 | C11A—C12A | 1.3900 |
N1—H6 | 0.9100 | C11A—H11A | 0.9500 |
C1—C2 | 1.506 (4) | C12A—C13A | 1.3900 |
C1—H10 | 0.9900 | C12A—H12A | 0.9500 |
C1—H11 | 0.9900 | C13A—C14A | 1.3900 |
C2—C7 | 1.384 (5) | C13A—H13A | 0.9500 |
C2—C3 | 1.385 (5) | C14A—H14A | 0.9500 |
C3—C4 | 1.398 (6) | C9B—C10B | 1.3900 |
C3—H12 | 0.9500 | C9B—C14B | 1.3900 |
C4—C5 | 1.369 (6) | C10B—C11B | 1.3900 |
C4—H13 | 0.9500 | C10B—H10B | 0.9500 |
C5—C6 | 1.367 (7) | C11B—C12B | 1.3900 |
C5—H14 | 0.9500 | C11B—H11B | 0.9500 |
C6—C7 | 1.389 (6) | C12B—C13B | 1.3900 |
C6—H15 | 0.9500 | C12B—H12B | 0.9500 |
C7—H16 | 0.9500 | C13B—C14B | 1.3900 |
N2—C8 | 1.487 (3) | C13B—H13B | 0.9500 |
N2—H7 | 0.9100 | C14B—H14B | 0.9500 |
N2—H8 | 0.9100 | O5—H2 | 0.9595 |
N2—H9 | 0.9100 | O5—H3 | 0.8499 |
C8—C9B | 1.4829 | ||
O1—As1—O2 | 112.66 (11) | N2—C8—C9A | 113.84 (11) |
O1—As1—O3 | 110.23 (11) | C9B—C8—H17 | 106.8 |
O2—As1—O3 | 110.89 (10) | N2—C8—H17 | 109.0 |
O1—As1—O4 | 109.09 (11) | C9A—C8—H17 | 110.1 |
O2—As1—O4 | 105.84 (10) | C9B—C8—H18 | 112.1 |
O3—As1—O4 | 107.92 (11) | N2—C8—H18 | 109.1 |
As1—O4—H1 | 113.0 | C9A—C8—H18 | 106.8 |
C1—N1—H4 | 109.5 | H17—C8—H18 | 107.8 |
C1—N1—H5 | 109.5 | C10A—C9A—C14A | 120.0 |
H4—N1—H5 | 109.5 | C10A—C9A—C8 | 120.9 |
C1—N1—H6 | 109.5 | C14A—C9A—C8 | 119.1 |
H4—N1—H6 | 109.5 | C11A—C10A—C9A | 120.0 |
H5—N1—H6 | 109.5 | C11A—C10A—H10A | 120.0 |
N1—C1—C2 | 111.8 (2) | C9A—C10A—H10A | 120.0 |
N1—C1—H10 | 109.3 | C10A—C11A—C12A | 120.0 |
C2—C1—H10 | 109.3 | C10A—C11A—H11A | 120.0 |
N1—C1—H11 | 109.3 | C12A—C11A—H11A | 120.0 |
C2—C1—H11 | 109.3 | C13A—C12A—C11A | 120.0 |
H10—C1—H11 | 107.9 | C13A—C12A—H12A | 120.0 |
C7—C2—C3 | 118.8 (3) | C11A—C12A—H12A | 120.0 |
C7—C2—C1 | 120.4 (3) | C14A—C13A—C12A | 120.0 |
C3—C2—C1 | 120.9 (3) | C14A—C13A—H13A | 120.0 |
C2—C3—C4 | 119.8 (4) | C12A—C13A—H13A | 120.0 |
C2—C3—H12 | 120.1 | C13A—C14A—C9A | 120.0 |
C4—C3—H12 | 120.1 | C13A—C14A—H14A | 120.0 |
C5—C4—C3 | 120.9 (4) | C9A—C14A—H14A | 120.0 |
C5—C4—H13 | 119.5 | C10B—C9B—C14B | 120.0 |
C3—C4—H13 | 119.5 | C10B—C9B—C8 | 118.6 |
C6—C5—C4 | 119.3 (4) | C14B—C9B—C8 | 121.4 |
C6—C5—H14 | 120.3 | C9B—C10B—C11B | 120.0 |
C4—C5—H14 | 120.3 | C9B—C10B—H10B | 120.0 |
C5—C6—C7 | 120.6 (4) | C11B—C10B—H10B | 120.0 |
C5—C6—H15 | 119.7 | C12B—C11B—C10B | 120.0 |
C7—C6—H15 | 119.7 | C12B—C11B—H11B | 120.0 |
C2—C7—C6 | 120.6 (4) | C10B—C11B—H11B | 120.0 |
C2—C7—H16 | 119.7 | C13B—C12B—C11B | 120.0 |
C6—C7—H16 | 119.7 | C13B—C12B—H12B | 120.0 |
C8—N2—H7 | 109.5 | C11B—C12B—H12B | 120.0 |
C8—N2—H8 | 109.5 | C12B—C13B—C14B | 120.0 |
H7—N2—H8 | 109.5 | C12B—C13B—H13B | 120.0 |
C8—N2—H9 | 109.5 | C14B—C13B—H13B | 120.0 |
H7—N2—H9 | 109.5 | C13B—C14B—C9B | 120.0 |
H8—N2—H9 | 109.5 | C13B—C14B—H14B | 120.0 |
C9B—C8—N2 | 111.92 (11) | C9B—C14B—H14B | 120.0 |
C9B—C8—C9A | 5.4 | H2—O5—H3 | 104.7 |
D—H···A | D—H | H···A | D···A | D—H···A |
O4—H1···O3i | 0.89 | 1.74 | 2.632 (3) | 173 |
N1—H4···O2ii | 0.91 | 1.94 | 2.830 (3) | 166 |
N1—H5···O2iii | 0.91 | 1.99 | 2.843 (3) | 155 |
N1—H6···O1 | 0.91 | 1.80 | 2.704 (3) | 174 |
N2—H7···O1iv | 0.91 | 1.86 | 2.731 (3) | 161 |
N2—H8···O5 | 0.91 | 1.92 | 2.823 (3) | 174 |
N2—H9···O3 | 0.91 | 1.94 | 2.835 (3) | 169 |
O5—H2···O3iii | 0.96 | 1.78 | 2.731 (3) | 171 |
O5—H3···O2ii | 0.85 | 1.98 | 2.825 (2) | 176 |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y, −z+1; (iii) x−1, y, z; (iv) −x+1, −y+1, −z+1. |
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