Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804013078/su6111sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804013078/su6111Isup2.hkl |
CCDC reference: 245118
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (Cr-O) = 0.003 Å
- R factor = 0.053
- wR factor = 0.149
- Data-to-parameter ratio = 18.1
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... N1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... N2 PLAT417_ALERT_2_C Short Inter D-H..H-D H3A .. H4A .. 2.12 Ang. PLAT417_ALERT_2_C Short Inter D-H..H-D H3A .. H4A .. 2.12 Ang. PLAT731_ALERT_1_C Bond Calc 0.83(4), Rep 0.833(19) ...... 2.11 su-Rat O2 -H2A 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT and SADABS (Sheldrick, 2002); program(s) used to solve structure: SHELXTL (Bruker, 2001); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 2000); software used to prepare material for publication: SHELXTL.
(C4H12N)2[CrCl2(H2O)4]Cl3·2H2O | F(000) = 1020 |
Mr = 485.64 | Dx = 1.392 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 8192 reflections |
a = 18.4374 (2) Å | θ = 2.2–27.3° |
b = 6.8192 (1) Å | µ = 1.09 mm−1 |
c = 18.4330 (2) Å | T = 173 K |
V = 2317.55 (5) Å3 | Plate, green |
Z = 4 | 0.20 × 0.08 × 0.04 mm |
Siemens SMART 1K CCD area-detector diffractometer | 2822 independent reflections |
Radiation source: fine-focus sealed tube | 2139 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.087 |
ω scans | θmax = 27.3°, θmin = 2.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2002) | h = −23→23 |
Tmin = 0.811, Tmax = 0.958 | k = −8→8 |
27823 measured reflections | l = −23→23 |
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)] = 0.053 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.149 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.09P)2 + 2.33P] where P = (Fo2 + 2Fc2)/3 |
2822 reflections | (Δ/σ)max = 0.001 |
156 parameters | Δρmax = 0.73 e Å−3 |
14 restraints | Δρmin = −0.59 e Å−3 |
Experimental. Data were collected at low temperature using a Siemens SMART CCD diffractometer equiped with an LT-2 device. A full sphere of reciprocal space was scanned by 0.3° steps in ω with a crystal-to-detector distance of 3.97 cm, 15 s per frame. Preliminary orientation matrix was obtained from the first 100 frames using SMART (Siemens, 1995). The collected frames were integrated using the preliminary orientation matrix which was updated every 100 frames. Final cell parameters were obtained by refinement on the position of 5499 reflections with I>10σ(I) after integration of all the frames data using SAINT (Siemens, 1995). |
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) | |
Cr1 | 0.71940 (4) | 0.2500 | 0.14394 (4) | 0.0169 (2) | |
Cl1 | 0.61233 (7) | 0.2500 | 0.07851 (7) | 0.0263 (3) | |
Cl2 | 0.82359 (7) | 0.2500 | 0.21146 (7) | 0.0270 (3) | |
Cl3 | 0.78375 (9) | 0.2500 | −0.06564 (7) | 0.0377 (4) | |
Cl4 | 0.55765 (7) | 0.7500 | 0.18657 (8) | 0.0280 (3) | |
Cl5 | 0.88503 (7) | 0.7500 | 0.07961 (7) | 0.0273 (3) | |
O1 | 0.75817 (14) | 0.0422 (4) | 0.07719 (13) | 0.0243 (6) | |
H1A | 0.791 (2) | −0.037 (6) | 0.090 (3) | 0.067 (18)* | |
H1B | 0.763 (2) | 0.081 (7) | 0.0341 (13) | 0.049 (15)* | |
O2 | 0.68020 (14) | 0.0414 (4) | 0.20859 (14) | 0.0239 (5) | |
H2A | 0.706 (2) | −0.044 (5) | 0.228 (2) | 0.044 (14)* | |
H2B | 0.6420 (15) | −0.018 (5) | 0.198 (2) | 0.024 (11)* | |
O3 | 0.4018 (2) | 0.7500 | 0.2518 (2) | 0.0466 (12) | |
H3A | 0.398 (4) | 0.7500 | 0.2981 (12) | 0.07 (3)* | |
H3B | 0.4439 (17) | 0.7500 | 0.233 (3) | 0.034 (17)* | |
O4 | 0.2583 (2) | 0.7500 | 0.2291 (2) | 0.0254 (8) | |
H4A | 0.3041 (11) | 0.7500 | 0.232 (4) | 0.05 (2)* | |
H4B | 0.246 (3) | 0.7500 | 0.1849 (14) | 0.04 (2)* | |
N1 | 0.0393 (2) | 0.2500 | 0.1310 (2) | 0.0285 (10) | |
N2 | 0.3874 (2) | 0.2500 | 0.0763 (2) | 0.0227 (9) | |
C11 | 0.0827 (3) | 0.0695 (9) | 0.1176 (3) | 0.0684 (16) | |
H11A | 0.1256 | 0.0699 | 0.1490 | 0.058 (5)* | |
H11B | 0.0980 | 0.0660 | 0.0667 | 0.058 (5)* | |
H11C | 0.0531 | −0.0463 | 0.1283 | 0.058 (5)* | |
C12 | −0.0235 (4) | 0.2500 | 0.0797 (3) | 0.0454 (16) | |
H12A | −0.0577 | 0.1463 | 0.0935 | 0.058 (5)* | 0.50 |
H12B | −0.0061 | 0.2264 | 0.0303 | 0.058 (5)* | 0.50 |
H12C | −0.0481 | 0.3774 | 0.0817 | 0.058 (5)* | 0.50 |
C13 | 0.0134 (4) | 0.2500 | 0.2076 (3) | 0.0398 (14) | |
H13A | 0.0549 | 0.2639 | 0.2404 | 0.058 (5)* | 0.50 |
H13B | −0.0117 | 0.1263 | 0.2178 | 0.058 (5)* | 0.50 |
H13C | −0.0201 | 0.3598 | 0.2150 | 0.058 (5)* | 0.50 |
C21 | 0.4163 (2) | 0.0711 (6) | 0.1126 (2) | 0.0386 (10) | |
H21A | 0.3991 | −0.0458 | 0.0869 | 0.058 (5)* | |
H21B | 0.3993 | 0.0673 | 0.1630 | 0.058 (5)* | |
H21C | 0.4694 | 0.0742 | 0.1118 | 0.058 (5)* | |
C22 | 0.4095 (4) | 0.2500 | −0.0016 (3) | 0.0410 (15) | |
H22A | 0.3984 | 0.3779 | −0.0231 | 0.058 (5)* | 0.50 |
H22B | 0.3828 | 0.1474 | −0.0275 | 0.058 (5)* | 0.50 |
H22C | 0.4617 | 0.2247 | −0.0052 | 0.058 (5)* | 0.50 |
C23 | 0.3066 (3) | 0.2500 | 0.0819 (4) | 0.0451 (16) | |
H23A | 0.2869 | 0.1377 | 0.0551 | 0.058 (5)* | 0.50 |
H23B | 0.2874 | 0.3718 | 0.0613 | 0.058 (5)* | 0.50 |
H23C | 0.2924 | 0.2404 | 0.1330 | 0.058 (5)* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr1 | 0.0190 (4) | 0.0129 (4) | 0.0189 (4) | 0.000 | −0.0017 (3) | 0.000 |
Cl1 | 0.0244 (6) | 0.0215 (6) | 0.0329 (7) | 0.000 | −0.0090 (5) | 0.000 |
Cl2 | 0.0222 (6) | 0.0317 (7) | 0.0271 (6) | 0.000 | −0.0068 (5) | 0.000 |
Cl3 | 0.0586 (10) | 0.0327 (7) | 0.0219 (7) | 0.000 | 0.0041 (6) | 0.000 |
Cl4 | 0.0224 (6) | 0.0222 (6) | 0.0396 (7) | 0.000 | 0.0014 (5) | 0.000 |
Cl5 | 0.0310 (7) | 0.0228 (6) | 0.0281 (7) | 0.000 | 0.0029 (5) | 0.000 |
O1 | 0.0340 (15) | 0.0193 (13) | 0.0195 (13) | 0.0043 (11) | −0.0020 (11) | −0.0022 (11) |
O2 | 0.0260 (14) | 0.0181 (12) | 0.0275 (13) | −0.0015 (11) | −0.0026 (11) | 0.0048 (11) |
O3 | 0.026 (2) | 0.081 (3) | 0.033 (2) | 0.000 | 0.008 (2) | 0.000 |
O4 | 0.026 (2) | 0.0254 (19) | 0.025 (2) | 0.000 | 0.0017 (16) | 0.000 |
N1 | 0.032 (2) | 0.026 (2) | 0.028 (2) | 0.000 | 0.0054 (19) | 0.000 |
N2 | 0.031 (2) | 0.021 (2) | 0.016 (2) | 0.000 | −0.0039 (17) | 0.000 |
C11 | 0.071 (2) | 0.070 (2) | 0.064 (2) | 0.0153 (17) | 0.0028 (17) | 0.0016 (17) |
C12 | 0.043 (4) | 0.053 (4) | 0.040 (4) | 0.000 | −0.007 (3) | 0.000 |
C13 | 0.048 (4) | 0.045 (4) | 0.026 (3) | 0.000 | 0.012 (3) | 0.000 |
C21 | 0.052 (3) | 0.026 (2) | 0.037 (2) | 0.0101 (19) | 0.001 (2) | 0.0077 (18) |
C22 | 0.068 (4) | 0.031 (3) | 0.024 (3) | 0.000 | 0.004 (3) | 0.000 |
C23 | 0.038 (3) | 0.055 (4) | 0.043 (4) | 0.000 | −0.015 (3) | 0.000 |
Cr1—O2i | 1.992 (2) | N2—C21 | 1.490 (4) |
Cr1—O2 | 1.992 (2) | N2—C21i | 1.490 (4) |
Cr1—O1i | 2.008 (3) | C11—H11A | 0.9800 |
Cr1—O1 | 2.008 (3) | C11—H11B | 0.9800 |
Cr1—Cl2 | 2.2889 (14) | C11—H11C | 0.9800 |
Cr1—Cl1 | 2.3133 (14) | C12—H12A | 0.9800 |
O1—H1A | 0.85 (2) | C12—H12B | 0.9800 |
O1—H1B | 0.842 (19) | C12—H12C | 0.9800 |
O2—H2A | 0.833 (19) | C13—H13A | 0.9800 |
O2—H2B | 0.838 (19) | C13—H13B | 0.9800 |
O3—H3A | 0.86 (2) | C13—H13C | 0.9800 |
O3—H3B | 0.85 (2) | C21—H21A | 0.9800 |
O4—H4A | 0.85 (2) | C21—H21B | 0.9800 |
O4—H4B | 0.85 (2) | C21—H21C | 0.9800 |
N1—C13 | 1.490 (7) | C22—H22A | 0.9800 |
N1—C11i | 1.489 (6) | C22—H22B | 0.9800 |
N1—C11 | 1.489 (6) | C22—H22C | 0.9800 |
N1—C12 | 1.496 (8) | C23—H23A | 0.9800 |
N2—C22 | 1.492 (7) | C23—H23B | 0.9800 |
N2—C23 | 1.494 (8) | C23—H23C | 0.9800 |
O2i—Cr1—O2 | 91.17 (15) | N1—C11—H11B | 109.5 |
O2i—Cr1—O1i | 89.52 (11) | H11A—C11—H11B | 109.5 |
O2—Cr1—O1i | 178.97 (11) | N1—C11—H11C | 109.5 |
O2i—Cr1—O1 | 178.97 (11) | H11A—C11—H11C | 109.5 |
O2—Cr1—O1 | 89.53 (11) | H11B—C11—H11C | 109.5 |
O1i—Cr1—O1 | 89.77 (15) | N1—C12—H12A | 109.5 |
O2i—Cr1—Cl2 | 88.81 (8) | N1—C12—H12B | 109.5 |
O2—Cr1—Cl2 | 88.81 (8) | H12A—C12—H12B | 109.5 |
O1i—Cr1—Cl2 | 91.98 (8) | N1—C12—H12C | 109.5 |
O1—Cr1—Cl2 | 91.97 (8) | H12A—C12—H12C | 109.5 |
O2i—Cr1—Cl1 | 90.13 (8) | H12B—C12—H12C | 109.5 |
O2—Cr1—Cl1 | 90.13 (8) | N1—C13—H13A | 109.5 |
O1i—Cr1—Cl1 | 89.10 (8) | N1—C13—H13B | 109.5 |
O1—Cr1—Cl1 | 89.10 (8) | H13A—C13—H13B | 109.5 |
Cl2—Cr1—Cl1 | 178.48 (6) | N1—C13—H13C | 109.5 |
Cr1—O1—H1A | 123 (4) | H13A—C13—H13C | 109.5 |
Cr1—O1—H1B | 114 (3) | H13B—C13—H13C | 109.5 |
H1A—O1—H1B | 112 (5) | N2—C21—H21A | 109.5 |
Cr1—O2—H2A | 123 (3) | N2—C21—H21B | 109.5 |
Cr1—O2—H2B | 120 (3) | H21A—C21—H21B | 109.5 |
H2A—O2—H2B | 104 (4) | N2—C21—H21C | 109.5 |
H3A—O3—H3B | 119 (7) | H21A—C21—H21C | 109.5 |
H4A—O4—H4B | 109 (6) | H21B—C21—H21C | 109.5 |
C13—N1—C11i | 109.2 (3) | N2—C22—H22A | 109.5 |
C13—N1—C11 | 109.2 (3) | N2—C22—H22B | 109.5 |
C11i—N1—C11 | 111.5 (5) | H22A—C22—H22B | 109.5 |
C13—N1—C12 | 110.5 (5) | N2—C22—H22C | 109.5 |
C11i—N1—C12 | 108.1 (3) | H22A—C22—H22C | 109.5 |
C11—N1—C12 | 108.2 (3) | H22B—C22—H22C | 109.5 |
C22—N2—C23 | 109.8 (5) | N2—C23—H23A | 109.5 |
C22—N2—C21 | 109.5 (3) | N2—C23—H23B | 109.5 |
C23—N2—C21 | 109.0 (3) | H23A—C23—H23B | 109.5 |
C22—N2—C21i | 109.6 (3) | N2—C23—H23C | 109.5 |
C23—N2—C21i | 109.0 (3) | H23A—C23—H23C | 109.5 |
C21—N2—C21i | 109.9 (4) | H23B—C23—H23C | 109.5 |
N1—C11—H11A | 109.5 |
Symmetry code: (i) x, −y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···Cl5ii | 0.85 (2) | 2.27 (3) | 3.073 (3) | 159 (5) |
O1—H1B···Cl3 | 0.84 (2) | 2.20 (2) | 3.027 (3) | 166 (5) |
O2—H2A···O4iii | 0.83 (2) | 1.88 (2) | 2.709 (3) | 175 (5) |
O2—H2B···Cl4ii | 0.84 (2) | 2.23 (2) | 3.036 (3) | 163 (4) |
O3—H3A···Cl5iv | 0.86 (2) | 2.27 (2) | 3.123 (5) | 178 (7) |
O3—H3B···Cl4 | 0.85 (2) | 2.26 (2) | 3.115 (4) | 177 (6) |
O4—H4A···O3 | 0.85 (2) | 1.84 (2) | 2.679 (6) | 172 (7) |
O4—H4B···Cl3v | 0.85 (2) | 2.27 (2) | 3.112 (4) | 178 (6) |
C12—H12C···Cl5vi | 0.98 | 2.82 | 3.803 (3) | 177 |
C22—H22A···Cl1v | 0.98 | 2.74 | 3.715 (2) | 172 |
Symmetry codes: (ii) x, y−1, z; (iii) x+1/2, −y+1/2, −z+1/2; (iv) x−1/2, −y+3/2, −z+1/2; (v) −x+1, y+1/2, −z; (vi) x−1, y, z. |
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