Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803027983/hg6011sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803027983/hg6011Isup2.hkl |
CCDC reference: 234802
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- H-atom completeness 97%
- Disorder in solvent or counterion
- R factor = 0.028
- wR factor = 0.083
- Data-to-parameter ratio = 26.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT420_ALERT_2_C D-H Without Acceptor N3 - H2N3 ... ? PLAT420_ALERT_2_C D-H Without Acceptor N5 - H2N5 ... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C8 H27 Mn1 N6 O0.5 S7 Sb4 Atom count from the _atom_site data: C8 H26 Mn1 N6 O0.5 S7 Sb4 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional? From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C8 H27 Mn N6 O0.5 S7 Sb4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 32.00 32.00 0.00 H 108.00 104.00 4.00 Mn 4.00 4.00 0.00 N 24.00 24.00 0.00 O 2.00 2.00 0.00 S 28.00 28.00 0.00 Sb 16.00 16.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS (Stoe & Cie, 1998); cell refinement: IPDS; data reduction: IPDS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Crystal Impact, 1999); software used to prepare material for publication: CIFTAB in SHELXL97.
[Mn(C4H13N3)2][Sb4S7]·0.5H20 | F(000) = 1844 |
Mr = 980.71 | Dx = 2.400 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8000 reflections |
a = 9.7216 (19) Å | θ = 2.5–28° |
b = 16.113 (3) Å | µ = 4.93 mm−1 |
c = 17.339 (4) Å | T = 293 K |
β = 91.88 (3)° | Polyhedra, yellow |
V = 2714.6 (9) Å3 | 0.2 × 0.2 × 0.1 mm |
Z = 4 |
Stoe IPDS diffractometer | 6508 independent reflections |
Radiation source: fine-focus sealed tube | 5824 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
φ scans | θmax = 28.0°, θmin = 2.5° |
Absorption correction: numerical [X-SHAPE (Stoe & Cie, 1998)and X-RED (Stoe & Cie, 1998)] | h = −12→12 |
Tmin = 0.390, Tmax = 0.609 | k = −21→21 |
31130 measured reflections | l = −22→22 |
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)] = 0.028 | H-atom parameters constrained |
wR(F2) = 0.083 | w = 1/[σ2(Fo2) + (0.0547P)2 + 3.6221P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
6508 reflections | Δρmax = 1.25 e Å−3 |
245 parameters | Δρmin = −1.12 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: 0.00169 (13) |
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) | |
Mn | 0.60094 (6) | 0.72629 (4) | 0.49237 (3) | 0.02702 (13) | |
Sb1 | −0.02292 (2) | 0.878909 (15) | 0.743886 (14) | 0.02171 (8) | |
Sb2 | 0.00953 (2) | 0.640658 (15) | 0.760134 (14) | 0.02201 (8) | |
Sb3 | 0.33220 (3) | 0.523731 (15) | 0.776720 (15) | 0.02592 (8) | |
Sb4 | 0.70681 (3) | 0.484698 (16) | 0.756691 (16) | 0.02626 (8) | |
S1 | 0.06567 (10) | 0.97071 (6) | 0.64786 (5) | 0.02589 (19) | |
S2 | −0.26679 (9) | 0.87910 (6) | 0.70261 (7) | 0.0300 (2) | |
S3 | 0.02577 (10) | 0.75440 (6) | 0.66536 (6) | 0.02764 (19) | |
S4 | −0.24192 (10) | 0.63188 (6) | 0.73701 (7) | 0.0330 (2) | |
S5 | 0.10328 (11) | 0.54262 (6) | 0.67292 (5) | 0.02722 (19) | |
S6 | 0.47357 (10) | 0.51326 (7) | 0.66700 (6) | 0.0279 (2) | |
S7 | 0.55817 (11) | 0.48663 (8) | 0.86381 (6) | 0.0338 (2) | |
N1 | 0.3699 (4) | 0.7394 (2) | 0.4727 (2) | 0.0344 (8) | |
H1N1 | 0.3476 | 0.7942 | 0.4724 | 0.041* | |
N2 | 0.5209 (4) | 0.7268 (2) | 0.61302 (19) | 0.0323 (7) | |
H1N2 | 0.5443 | 0.6789 | 0.6367 | 0.039* | |
H2N2 | 0.5605 | 0.7687 | 0.6400 | 0.039* | |
N3 | 0.5700 (5) | 0.7161 (3) | 0.3595 (2) | 0.0440 (10) | |
H1N3 | 0.6272 | 0.7515 | 0.3363 | 0.053* | |
H2N3 | 0.5900 | 0.6643 | 0.3441 | 0.053* | |
N4 | 0.8302 (4) | 0.7126 (3) | 0.5034 (2) | 0.0353 (8) | |
H1N4 | 0.8562 | 0.7178 | 0.5540 | 0.042* | |
N5 | 0.6752 (5) | 0.8591 (3) | 0.4887 (3) | 0.0484 (11) | |
H1N5 | 0.6410 | 0.8839 | 0.4457 | 0.058* | |
H2N5 | 0.6445 | 0.8869 | 0.5297 | 0.058* | |
N6 | 0.6385 (4) | 0.5839 (2) | 0.5000 (2) | 0.0404 (9) | |
H1N6 | 0.5885 | 0.5624 | 0.5379 | 0.049* | |
H2N6 | 0.6109 | 0.5599 | 0.4553 | 0.049* | |
C1 | 0.3070 (4) | 0.6994 (4) | 0.5388 (3) | 0.0421 (11) | |
H1A | 0.3238 | 0.6401 | 0.5376 | 0.051* | |
H1B | 0.2083 | 0.7085 | 0.5367 | 0.051* | |
C2 | 0.3700 (5) | 0.7366 (3) | 0.6128 (3) | 0.0387 (10) | |
H2A | 0.3466 | 0.7950 | 0.6158 | 0.046* | |
H2B | 0.3335 | 0.7087 | 0.6572 | 0.046* | |
C3 | 0.3309 (5) | 0.7030 (4) | 0.3969 (3) | 0.0484 (12) | |
H3A | 0.2363 | 0.7172 | 0.3830 | 0.058* | |
H3B | 0.3384 | 0.6430 | 0.3993 | 0.058* | |
C4 | 0.4253 (6) | 0.7364 (3) | 0.3369 (3) | 0.0501 (13) | |
H4A | 0.4018 | 0.7119 | 0.2871 | 0.060* | |
H4B | 0.4143 | 0.7960 | 0.3327 | 0.060* | |
C5 | 0.8881 (6) | 0.7827 (4) | 0.4606 (3) | 0.0508 (13) | |
H5A | 0.8657 | 0.7767 | 0.4060 | 0.061* | |
H5B | 0.9875 | 0.7832 | 0.4676 | 0.061* | |
C6 | 0.8302 (6) | 0.8619 (4) | 0.4894 (3) | 0.0551 (15) | |
H6A | 0.8597 | 0.9074 | 0.4572 | 0.066* | |
H6B | 0.8651 | 0.8721 | 0.5416 | 0.066* | |
C7 | 0.8704 (6) | 0.6294 (4) | 0.4768 (3) | 0.0524 (13) | |
H7A | 0.9672 | 0.6199 | 0.4890 | 0.063* | |
H7B | 0.8560 | 0.6253 | 0.4213 | 0.063* | |
C8 | 0.7857 (6) | 0.5659 (3) | 0.5157 (3) | 0.0505 (13) | |
H8A | 0.8077 | 0.5110 | 0.4966 | 0.061* | |
H8B | 0.8057 | 0.5669 | 0.5709 | 0.061* | |
O | 0.2287 (9) | 0.9120 (4) | 0.4739 (4) | 0.0513 (19) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn | 0.0255 (3) | 0.0309 (3) | 0.0247 (3) | −0.0044 (2) | 0.0019 (2) | 0.0010 (2) |
Sb1 | 0.01879 (12) | 0.02100 (13) | 0.02533 (13) | −0.00158 (8) | 0.00089 (9) | 0.00326 (8) |
Sb2 | 0.01717 (12) | 0.02230 (13) | 0.02644 (13) | 0.00324 (8) | −0.00115 (9) | −0.00453 (9) |
Sb3 | 0.02609 (14) | 0.01968 (13) | 0.03232 (14) | −0.00045 (9) | 0.00612 (10) | −0.00277 (9) |
Sb4 | 0.02345 (14) | 0.02348 (14) | 0.03193 (14) | 0.00115 (9) | 0.00196 (10) | −0.00429 (9) |
S1 | 0.0288 (5) | 0.0228 (4) | 0.0261 (4) | −0.0084 (3) | 0.0013 (4) | 0.0024 (3) |
S2 | 0.0163 (4) | 0.0249 (4) | 0.0490 (6) | −0.0016 (3) | 0.0031 (4) | −0.0140 (4) |
S3 | 0.0301 (5) | 0.0190 (4) | 0.0344 (5) | 0.0039 (3) | 0.0097 (4) | 0.0003 (3) |
S4 | 0.0166 (4) | 0.0280 (5) | 0.0541 (6) | 0.0013 (3) | −0.0018 (4) | 0.0122 (4) |
S5 | 0.0348 (5) | 0.0206 (4) | 0.0264 (4) | 0.0085 (4) | 0.0032 (4) | −0.0002 (3) |
S6 | 0.0203 (4) | 0.0389 (5) | 0.0246 (4) | −0.0053 (4) | 0.0017 (3) | 0.0040 (4) |
S7 | 0.0218 (5) | 0.0524 (7) | 0.0271 (5) | −0.0061 (4) | −0.0007 (4) | 0.0058 (4) |
N1 | 0.0334 (18) | 0.040 (2) | 0.0293 (17) | 0.0078 (15) | −0.0049 (14) | −0.0066 (14) |
N2 | 0.0289 (17) | 0.042 (2) | 0.0261 (15) | −0.0044 (15) | −0.0011 (13) | −0.0004 (14) |
N3 | 0.057 (3) | 0.050 (2) | 0.0258 (17) | −0.004 (2) | 0.0060 (17) | −0.0025 (16) |
N4 | 0.0315 (18) | 0.043 (2) | 0.0313 (17) | −0.0065 (16) | 0.0030 (14) | 0.0007 (15) |
N5 | 0.065 (3) | 0.031 (2) | 0.049 (2) | −0.0066 (19) | −0.008 (2) | 0.0079 (17) |
N6 | 0.055 (2) | 0.033 (2) | 0.0336 (18) | −0.0110 (18) | 0.0054 (17) | −0.0027 (15) |
C1 | 0.023 (2) | 0.065 (3) | 0.039 (2) | −0.004 (2) | 0.0020 (17) | −0.010 (2) |
C2 | 0.030 (2) | 0.056 (3) | 0.0300 (19) | 0.001 (2) | 0.0044 (16) | −0.0071 (19) |
C3 | 0.040 (3) | 0.069 (4) | 0.036 (2) | 0.006 (2) | −0.013 (2) | −0.010 (2) |
C4 | 0.074 (4) | 0.049 (3) | 0.027 (2) | 0.008 (3) | −0.010 (2) | 0.0030 (19) |
C5 | 0.040 (3) | 0.068 (4) | 0.045 (3) | −0.019 (3) | 0.008 (2) | 0.012 (3) |
C6 | 0.070 (4) | 0.048 (3) | 0.047 (3) | −0.031 (3) | −0.001 (3) | 0.013 (2) |
C7 | 0.042 (3) | 0.057 (3) | 0.059 (3) | 0.006 (2) | 0.012 (2) | −0.012 (3) |
C8 | 0.067 (3) | 0.038 (3) | 0.047 (3) | 0.012 (2) | 0.001 (2) | −0.004 (2) |
O | 0.088 (6) | 0.039 (4) | 0.027 (3) | 0.024 (4) | 0.012 (3) | −0.013 (3) |
Mn—N4 | 2.241 (4) | N3—H2N3 | 0.9000 |
Mn—N2 | 2.256 (4) | N4—C5 | 1.473 (6) |
Mn—N5 | 2.259 (4) | N4—C7 | 1.476 (7) |
Mn—N1 | 2.270 (4) | N4—H1N4 | 0.9100 |
Mn—N3 | 2.320 (4) | N5—C6 | 1.507 (8) |
Mn—N6 | 2.326 (4) | N5—H1N5 | 0.9000 |
Sb1—S1 | 2.4076 (10) | N5—H2N5 | 0.9000 |
Sb1—S2 | 2.4539 (11) | N6—C8 | 1.477 (7) |
Sb1—S3 | 2.4790 (10) | N6—H1N6 | 0.9000 |
Sb2—S5 | 2.3883 (10) | N6—H2N6 | 0.9000 |
Sb2—S4 | 2.4682 (11) | C1—C2 | 1.526 (6) |
Sb2—S3 | 2.4701 (10) | C1—H1A | 0.9700 |
Sb3—S6 | 2.3893 (12) | C1—H1B | 0.9700 |
Sb3—S2i | 2.4451 (11) | C2—H2A | 0.9700 |
Sb3—S7 | 2.6917 (13) | C2—H2B | 0.9700 |
Sb3—S5 | 2.8322 (13) | C3—C4 | 1.507 (8) |
Sb4—S7 | 2.3907 (13) | C3—H3A | 0.9700 |
Sb4—S4ii | 2.4495 (11) | C3—H3B | 0.9700 |
Sb4—S1iii | 2.7279 (13) | C4—H4A | 0.9700 |
Sb4—S6 | 2.7459 (13) | C4—H4B | 0.9700 |
S1—Sb4iv | 2.7279 (13) | C5—C6 | 1.487 (9) |
S2—Sb3v | 2.4451 (11) | C5—H5A | 0.9700 |
S4—Sb4vi | 2.4495 (11) | C5—H5B | 0.9700 |
N1—C1 | 1.466 (6) | C6—H6A | 0.9700 |
N1—C3 | 1.479 (5) | C6—H6B | 0.9700 |
N1—H1N1 | 0.9100 | C7—C8 | 1.489 (8) |
N2—C2 | 1.475 (6) | C7—H7A | 0.9700 |
N2—H1N2 | 0.9000 | C7—H7B | 0.9700 |
N2—H2N2 | 0.9000 | C8—H8A | 0.9700 |
N3—C4 | 1.484 (7) | C8—H8B | 0.9700 |
N3—H1N3 | 0.9000 | ||
N4—Mn—N2 | 107.09 (13) | C7—N4—H1N4 | 108.5 |
N4—Mn—N5 | 77.15 (16) | Mn—N4—H1N4 | 108.5 |
N2—Mn—N5 | 98.22 (16) | C6—N5—Mn | 110.4 (3) |
N4—Mn—N1 | 176.26 (13) | C6—N5—H1N5 | 109.6 |
N2—Mn—N1 | 76.64 (13) | Mn—N5—H1N5 | 109.6 |
N5—Mn—N1 | 102.89 (16) | C6—N5—H2N5 | 109.6 |
N4—Mn—N3 | 100.00 (15) | Mn—N5—H2N5 | 109.6 |
N2—Mn—N3 | 152.13 (15) | H1N5—N5—H2N5 | 108.1 |
N5—Mn—N3 | 93.99 (16) | C8—N6—Mn | 110.8 (3) |
N1—Mn—N3 | 76.26 (15) | C8—N6—H1N6 | 109.5 |
N4—Mn—N6 | 75.19 (15) | Mn—N6—H1N6 | 109.5 |
N2—Mn—N6 | 90.53 (14) | C8—N6—H2N6 | 109.5 |
N5—Mn—N6 | 152.33 (17) | Mn—N6—H2N6 | 109.5 |
N1—Mn—N6 | 104.66 (15) | H1N6—N6—H2N6 | 108.1 |
N3—Mn—N6 | 90.12 (15) | N1—C1—C2 | 108.5 (4) |
S1—Sb1—S2 | 99.30 (4) | N1—C1—H1A | 110.0 |
S1—Sb1—S3 | 92.19 (4) | C2—C1—H1A | 110.0 |
S2—Sb1—S3 | 92.35 (4) | N1—C1—H1B | 110.0 |
S5—Sb2—S4 | 104.82 (4) | C2—C1—H1B | 110.0 |
S5—Sb2—S3 | 92.03 (4) | H1A—C1—H1B | 108.4 |
S4—Sb2—S3 | 91.09 (4) | N2—C2—C1 | 109.4 (4) |
S6—Sb3—S2i | 102.04 (4) | N2—C2—H2A | 109.8 |
S6—Sb3—S7 | 87.18 (4) | C1—C2—H2A | 109.8 |
S2i—Sb3—S7 | 85.27 (4) | N2—C2—H2B | 109.8 |
S6—Sb3—S5 | 87.83 (4) | C1—C2—H2B | 109.8 |
S2i—Sb3—S5 | 89.59 (3) | H2A—C2—H2B | 108.2 |
S7—Sb3—S5 | 171.94 (3) | N1—C3—C4 | 109.1 (4) |
S7—Sb4—S4ii | 103.10 (4) | N1—C3—H3A | 109.9 |
S7—Sb4—S1iii | 91.63 (4) | C4—C3—H3A | 109.9 |
S4ii—Sb4—S1iii | 89.99 (3) | N1—C3—H3B | 109.9 |
S7—Sb4—S6 | 85.92 (4) | C4—C3—H3B | 109.9 |
S4ii—Sb4—S6 | 85.80 (3) | H3A—C3—H3B | 108.3 |
S1iii—Sb4—S6 | 174.53 (3) | N3—C4—C3 | 109.5 (4) |
Sb1—S1—Sb4iv | 86.13 (3) | N3—C4—H4A | 109.8 |
Sb3v—S2—Sb1 | 102.23 (3) | C3—C4—H4A | 109.8 |
Sb2—S3—Sb1 | 102.56 (4) | N3—C4—H4B | 109.8 |
Sb4vi—S4—Sb2 | 103.76 (4) | C3—C4—H4B | 109.8 |
Sb2—S5—Sb3 | 88.68 (3) | H4A—C4—H4B | 108.2 |
Sb3—S6—Sb4 | 92.68 (4) | N4—C5—C6 | 109.5 (4) |
Sb4—S7—Sb3 | 94.02 (4) | N4—C5—H5A | 109.8 |
C1—N1—C3 | 114.8 (4) | C6—C5—H5A | 109.8 |
C1—N1—Mn | 106.2 (3) | N4—C5—H5B | 109.8 |
C3—N1—Mn | 108.7 (3) | C6—C5—H5B | 109.8 |
C1—N1—H1N1 | 109.0 | H5A—C5—H5B | 108.2 |
C3—N1—H1N1 | 109.0 | C5—C6—N5 | 111.1 (4) |
Mn—N1—H1N1 | 109.0 | C5—C6—H6A | 109.4 |
C2—N2—Mn | 111.8 (2) | N5—C6—H6A | 109.4 |
C2—N2—H1N2 | 109.3 | C5—C6—H6B | 109.4 |
Mn—N2—H1N2 | 109.3 | N5—C6—H6B | 109.4 |
C2—N2—H2N2 | 109.3 | H6A—C6—H6B | 108.0 |
Mn—N2—H2N2 | 109.3 | N4—C7—C8 | 109.1 (4) |
H1N2—N2—H2N2 | 107.9 | N4—C7—H7A | 109.9 |
C4—N3—Mn | 109.7 (3) | C8—C7—H7A | 109.9 |
C4—N3—H1N3 | 109.7 | N4—C7—H7B | 109.9 |
Mn—N3—H1N3 | 109.7 | C8—C7—H7B | 109.9 |
C4—N3—H2N3 | 109.7 | H7A—C7—H7B | 108.3 |
Mn—N3—H2N3 | 109.7 | N6—C8—C7 | 109.1 (4) |
H1N3—N3—H2N3 | 108.2 | N6—C8—H8A | 109.9 |
C5—N4—C7 | 115.5 (4) | C7—C8—H8A | 109.9 |
C5—N4—Mn | 106.1 (3) | N6—C8—H8B | 109.9 |
C7—N4—Mn | 109.6 (3) | C7—C8—H8B | 109.9 |
C5—N4—H1N4 | 108.5 | H8A—C8—H8B | 108.3 |
Symmetry codes: (i) −x, y−1/2, −z+3/2; (ii) x+1, y, z; (iii) −x+1, y−1/2, −z+3/2; (iv) −x+1, y+1/2, −z+3/2; (v) −x, y+1/2, −z+3/2; (vi) x−1, y, z. |