Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102004080/ln1136sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102004080/ln1136Isup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102004080/ln1136IIsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102004080/ln1136IIIsup4.hkl |
CCDC references: 184508; 184509; 184510
Data collection: IPDS (Stoe & Cie, 1996) for (I), (II); IPDS (Stoe& Cie, 1996) for (III). For all compounds, cell refinement: IPDS; data reduction: IPDS. Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990) for (I), (III); SHELXS86 (Sheldrick, 1990) for (II). For all compounds, program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.
C14H15ClP2S2 | F(000) = 712 |
Mr = 344.77 | Dx = 1.472 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 13.204 (1) Å | Cell parameters from 5000 reflections |
b = 9.694 (1) Å | θ = 6.9–28.3° |
c = 13.655 (1) Å | µ = 0.70 mm−1 |
β = 117.11 (1)° | T = 190 K |
V = 1555.8 (3) Å3 | Prismatic, colourless |
Z = 4 | 0.57 × 0.38 × 0.19 mm |
Stoe IPDS diffractometer | 3738 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 3485 reflections with I > 2σ(I) |
Planar graphite monochromator | Rint = 0.043 |
Detector resolution: 6.667 pixels mm-1 | θmax = 28.1°, θmin = 2.7° |
φ scans | h = −17→15 |
Absorption correction: part of the refinement model (ΔF) (ABSCOR; Stoe & Cie, 1996) | k = −12→12 |
Tmin = 0.659, Tmax = 0.875 | l = −17→17 |
18747 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) = 0.081 | H-atom parameters constrained |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0507P)2 + 0.4476P] where P = (Fo2 + 2Fc2)/3 |
3738 reflections | (Δ/σ)max = 0.002 |
172 parameters | Δρmax = 0.41 e Å−3 |
0 restraints | Δρmin = −0.37 e Å−3 |
Experimental. Recrystallized from benzene. During data collection the crystal was in cold N2 gas of the Cryostream Cooler (Oxford Cryosystems, 1992) mounted on a φ-axis diffractometer supplied with an area detector. Data collection: φ-scans, φ-incr.=1.2 °, 200 exposures |
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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factors 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 | ||
P1 | 0.57851 (2) | 0.33775 (3) | 0.80861 (2) | 0.01820 (9) | |
C11 | 0.59187 (11) | 0.24627 (14) | 0.69960 (11) | 0.0253 (3) | |
H11A | 0.59616 | 0.14616 | 0.71535 | 0.030* | |
H11B | 0.52231 | 0.26257 | 0.62973 | 0.030* | |
C21 | 0.69530 (12) | 0.2873 (2) | 0.68391 (12) | 0.0311 (3) | |
H21A | 0.69630 | 0.2333 | 0.62367 | 0.037* | |
H21B | 0.76496 | 0.2691 | 0.75189 | 0.037* | |
H21C | 0.69098 | 0.3858 | 0.66612 | 0.037* | |
C12 | 0.55253 (10) | 0.51783 (13) | 0.77587 (10) | 0.0198 (2) | |
C22 | 0.52019 (10) | 0.56438 (14) | 0.66855 (10) | 0.0241 (2) | |
H22 | 0.51341 | 0.50105 | 0.61279 | 0.029* | |
C32 | 0.49810 (12) | 0.7036 (2) | 0.64411 (12) | 0.0291 (3) | |
H32 | 0.47656 | 0.7356 | 0.57152 | 0.035* | |
C42 | 0.50735 (12) | 0.79576 (14) | 0.72500 (13) | 0.0293 (3) | |
H42 | 0.49124 | 0.89068 | 0.70756 | 0.035* | |
C52 | 0.54016 (12) | 0.75017 (15) | 0.83193 (12) | 0.0294 (3) | |
H52 | 0.54697 | 0.81406 | 0.88735 | 0.035* | |
C62 | 0.56288 (11) | 0.61172 (14) | 0.85752 (11) | 0.0256 (3) | |
H62 | 0.58547 | 0.58063 | 0.93053 | 0.031* | |
C13 | 0.46268 (10) | 0.26518 (13) | 0.82703 (10) | 0.0215 (2) | |
C23 | 0.46365 (12) | 0.12464 (14) | 0.85078 (12) | 0.0281 (3) | |
H23 | 0.52279 | 0.06686 | 0.85303 | 0.034* | |
C33 | 0.37785 (12) | 0.0700 (2) | 0.87103 (12) | 0.0315 (3) | |
H33 | 0.37799 | −0.0255 | 0.88671 | 0.038* | |
C43 | 0.29182 (12) | 0.1546 (2) | 0.86842 (12) | 0.0303 (3) | |
H43 | 0.23350 | 0.1169 | 0.88278 | 0.036* | |
C53 | 0.29073 (11) | 0.2935 (2) | 0.84498 (12) | 0.0296 (3) | |
H53 | 0.23177 | 0.3510 | 0.84350 | 0.036* | |
C63 | 0.37566 (11) | 0.34947 (14) | 0.82356 (11) | 0.0251 (3) | |
H63 | 0.37431 | 0.44472 | 0.80664 | 0.030* | |
P2 | 0.74202 (3) | 0.30647 (4) | 0.96374 (3) | 0.02250 (9) | |
Cl2 | 0.67714 (3) | 0.34038 (4) | 1.07421 (3) | 0.03474 (10) | |
S12 | 0.84799 (3) | 0.45134 (4) | 0.97461 (3) | 0.03541 (11) | |
S22 | 0.77716 (3) | 0.11146 (4) | 0.96454 (3) | 0.03167 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
P1 | 0.01792 (15) | 0.0192 (2) | 0.0192 (2) | 0.00010 (10) | 0.00992 (12) | −0.00047 (11) |
C11 | 0.0277 (6) | 0.0260 (6) | 0.0250 (6) | −0.0018 (5) | 0.0144 (5) | −0.0059 (5) |
C21 | 0.0299 (6) | 0.0394 (8) | 0.0309 (7) | 0.0020 (6) | 0.0198 (6) | −0.0027 (6) |
C12 | 0.0182 (5) | 0.0210 (5) | 0.0212 (5) | −0.0002 (4) | 0.0097 (4) | 0.0006 (4) |
C22 | 0.0225 (6) | 0.0283 (6) | 0.0206 (6) | −0.0005 (5) | 0.0092 (5) | 0.0012 (5) |
C32 | 0.0280 (6) | 0.0325 (7) | 0.0256 (6) | 0.0015 (5) | 0.0112 (5) | 0.0079 (5) |
C42 | 0.0274 (6) | 0.0233 (6) | 0.0366 (7) | 0.0026 (5) | 0.0141 (5) | 0.0063 (5) |
C52 | 0.0348 (7) | 0.0238 (6) | 0.0312 (7) | 0.0024 (5) | 0.0165 (6) | −0.0018 (5) |
C62 | 0.0307 (6) | 0.0247 (6) | 0.0233 (6) | 0.0029 (5) | 0.0140 (5) | 0.0010 (5) |
C13 | 0.0206 (5) | 0.0231 (6) | 0.0225 (6) | −0.0022 (4) | 0.0115 (4) | −0.0007 (5) |
C23 | 0.0262 (6) | 0.0234 (6) | 0.0361 (7) | −0.0004 (5) | 0.0154 (5) | 0.0009 (5) |
C33 | 0.0317 (7) | 0.0273 (7) | 0.0352 (7) | −0.0058 (5) | 0.0150 (6) | 0.0043 (6) |
C43 | 0.0271 (6) | 0.0395 (8) | 0.0282 (7) | −0.0086 (6) | 0.0161 (5) | −0.0011 (6) |
C53 | 0.0246 (6) | 0.0355 (7) | 0.0336 (7) | −0.0008 (5) | 0.0175 (5) | −0.0028 (6) |
C63 | 0.0230 (6) | 0.0251 (6) | 0.0301 (6) | 0.0004 (5) | 0.0145 (5) | −0.0006 (5) |
P2 | 0.0219 (2) | 0.0232 (2) | 0.0205 (2) | 0.00246 (11) | 0.00795 (12) | 0.00144 (11) |
Cl2 | 0.0459 (2) | 0.0393 (2) | 0.0236 (2) | 0.00746 (15) | 0.01980 (15) | 0.00098 (13) |
S12 | 0.0257 (2) | 0.0314 (2) | 0.0414 (2) | −0.00534 (13) | 0.00848 (15) | 0.00362 (15) |
S22 | 0.0319 (2) | 0.0238 (2) | 0.0395 (2) | 0.00751 (12) | 0.01640 (15) | 0.00435 (14) |
P1—C12 | 1.7958 (13) | P2—S22 | 1.9454 (5) |
P1—C13 | 1.8023 (12) | P2—Cl2 | 2.0724 (5) |
P1—C11 | 1.8090 (13) | C11—H11A | 0.990 |
P1—P2 | 2.2522 (5) | C11—H11B | 0.990 |
C11—C21 | 1.528 (2) | C21—H21A | 0.980 |
C12—C62 | 1.397 (2) | C21—H21B | 0.980 |
C12—C22 | 1.401 (2) | C21—H21C | 0.980 |
C22—C32 | 1.389 (2) | C22—H22 | 0.950 |
C32—C42 | 1.382 (2) | C23—H23 | 0.950 |
C42—C52 | 1.392 (2) | C32—H32 | 0.950 |
C52—C62 | 1.385 (2) | C33—H33 | 0.950 |
C13—C63 | 1.393 (2) | C42—H42 | 0.950 |
C13—C23 | 1.399 (2) | C43—H43 | 0.950 |
C23—C33 | 1.388 (2) | C52—H52 | 0.950 |
C33—C43 | 1.388 (2) | C53—H53 | 0.950 |
C43—C53 | 1.383 (2) | C62—H62 | 0.950 |
C53—C63 | 1.392 (2) | C63—H63 | 0.950 |
P2—S12 | 1.9399 (5) | ||
C12—P1—C13 | 109.64 (6) | P1—C11—H11A | 108.6 |
C12—P1—C11 | 110.54 (6) | C21—C11—H11B | 108.8 |
C13—P1—C11 | 109.31 (6) | P1—C11—H11B | 108.6 |
C12—P1—P2 | 110.95 (4) | H11A—C11—H11B | 107.6 |
C13—P1—P2 | 109.08 (4) | C11—C21—H21A | 109.5 |
C11—P1—P2 | 107.27 (5) | C11—C21—H21B | 109.7 |
C21—C11—P1 | 114.59 (10) | H21A—C21—H21B | 109.4 |
C62—C12—C22 | 119.82 (12) | C11—C21—H21C | 109.4 |
C62—C12—P1 | 119.77 (10) | H21A—C21—H21C | 109.4 |
C22—C12—P1 | 120.40 (10) | H21B—C21—H21C | 109.4 |
C32—C22—C12 | 119.66 (12) | C32—C22—H22 | 120.5 |
C42—C32—C22 | 120.25 (13) | C12—C22—H22 | 119.9 |
C32—C42—C52 | 120.31 (13) | C33—C23—H23 | 120.0 |
C62—C52—C42 | 120.03 (13) | C13—C23—H23 | 120.2 |
C52—C62—C12 | 119.92 (12) | C42—C32—H32 | 119.9 |
C63—C13—C23 | 119.97 (12) | C22—C32—H32 | 119.5 |
C63—C13—P1 | 120.37 (10) | C23—C33—H33 | 120.1 |
C23—C13—P1 | 119.58 (10) | C43—C33—H33 | 119.6 |
C33—C23—C13 | 119.71 (13) | C32—C42—H42 | 119.8 |
C23—C33—C43 | 120.16 (14) | C52—C42—H42 | 119.8 |
C53—C43—C33 | 120.20 (12) | C53—C43—H43 | 119.9 |
C43—C53—C63 | 120.27 (13) | C33—C43—H43 | 120.3 |
C53—C63—C13 | 119.69 (13) | C62—C52—H52 | 120.1 |
S12—P2—S22 | 122.76 (2) | C42—C52—H52 | 120.0 |
S12—P2—Cl2 | 110.64 (2) | C43—C53—H53 | 119.9 |
S22—P2—Cl2 | 109.07 (2) | C63—C53—H53 | 120.5 |
S12—P2—P1 | 108.87 (2) | C52—C62—H62 | 119.9 |
S22—P2—P1 | 105.08 (2) | C12—C62—H62 | 120.3 |
Cl2—P2—P1 | 97.25 (2) | C53—C63—H63 | 119.6 |
C21—C11—H11A | 108.5 | C13—C63—H63 | 120.1 |
C9H21ClP2S2 | Melting point: 324 (decomp.) K |
Mr = 290.77 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3c1 | Cell parameters from 5000 reflections |
a = 11.413 (3) Å | θ = 2.5–25.0° |
c = 13.566 (3) Å | µ = 0.70 mm−1 |
V = 1530.3 (8) Å3 | T = 180 K |
Z = 4 | Block, colourless |
F(000) = 616 | 0.68 × 0.40 × 0.28 mm |
Dx = 1.262 Mg m−3 |
Stoe IPDS diffractometer | 1001 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 987 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
Detector resolution: 6.667 pixels mm-1 | θmax = 26.0°, θmin = 2.6° |
φ scans | h = −13→14 |
Absorption correction: numerical [XRED (Stoe & Cie, 1996) and XSHAPE (Stoe & Cie, 1996) based on HABITUS (Herrendorf, 1993)] | k = −14→13 |
Tmin = 0.777, Tmax = 0.848 | l = −16→16 |
10448 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)] = 0.022 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0313P)2 + 0.2298P] where P = (Fo2 + 2Fc2)/3 |
1000 reflections | (Δ/σ)max = 0.002 |
48 parameters | Δρmax = 0.30 e Å−3 |
2 restraints | Δρmin = −0.18 e Å−3 |
Experimental. Recrystallized from acetonitrile/benzene (1/10). During data collection the crystal was in cold N2 gas of the Cryostream Cooler (Oxford Cryosystems, 1992) mounted on a φ-axis diffractometer supplied with an area detector. Data collection: φ-scans, φ-incr.=1.5 °, 147 exposures |
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 on F2 for ALL reflections except for 1 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factors 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) | |
C1 | 0.79078 (15) | 0.49784 (15) | 0.65083 (11) | 0.0215 (3) | |
H1A | 0.87961 | 0.52214 | 0.68000 | 0.026* | |
H1B | 0.79849 | 0.49136 | 0.57859 | 0.026* | |
C2 | 0.7617 (2) | 0.6123 (2) | 0.67198 (14) | 0.0315 (4) | |
H2A | 0.6720 | 0.5886 | 0.64473 | 0.038* | |
H2B | 0.7591 | 0.6238 | 0.74413 | 0.038* | |
C3 | 0.8691 (2) | 0.7438 (2) | 0.6266 (2) | 0.0477 (5) | |
H3A | 0.8493 | 0.8160 | 0.6421 | 0.057* | |
H3B | 0.8697 | 0.7333 | 0.5550 | 0.057* | |
H3C | 0.9579 | 0.7671 | 0.6535 | 0.057* | |
P1 | 0.6667 | 0.3333 | 0.69654 (4) | 0.01700 (14) | |
P2 | 0.6667 | 0.3333 | 0.86057 (5) | 0.0273 (2) | |
S1 | 0.8512 (6) | 0.4661 (8) | 0.9020 (5) | 0.0319 (6) | 0.66667 |
Cl1 | 0.8609 (12) | 0.4746 (16) | 0.8906 (10) | 0.0319 (6) | 0.33333 |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0205 (7) | 0.0184 (7) | 0.0214 (7) | 0.0067 (5) | 0.0038 (5) | 0.0021 (5) |
C2 | 0.0319 (8) | 0.0223 (7) | 0.0412 (9) | 0.0142 (7) | 0.0066 (7) | 0.0042 (7) |
C3 | 0.0498 (11) | 0.0242 (8) | 0.064 (2) | 0.0146 (8) | 0.0115 (10) | 0.0138 (9) |
P1 | 0.0173 (2) | 0.0173 (2) | 0.0164 (3) | 0.00866 (9) | 0.000 | 0.000 |
P2 | 0.0333 (2) | 0.0333 (2) | 0.0153 (3) | 0.01664 (11) | 0.000 | 0.000 |
S1 | 0.0201 (8) | 0.0373 (10) | 0.022 (2) | 0.0024 (7) | 0.0013 (8) | 0.0008 (10) |
Cl1 | 0.0201 (8) | 0.0373 (10) | 0.022 (2) | 0.0024 (7) | 0.0013 (8) | 0.0008 (10) |
C1—C2 | 1.528 (2) | C3—H3A | 0.98 |
C1—P1 | 1.805 (2) | C3—H3B | 0.98 |
C1—H1A | 0.99 | C3—H3C | 0.98 |
C1—H1B | 0.99 | P1—P2 | 2.2253 (10) |
C2—C3 | 1.514 (2) | P2—S1 | 1.964 (6) |
C2—H2A | 0.99 | P2—Cl1 | 2.026 (12) |
C2—H2B | 0.99 | ||
C2—C1—P1 | 115.60 (11) | C2—C3—H3B | 109.47 |
C2—C1—H1A | 108.38 | H3A—C3—H3B | 109.5 |
P1—C1—H1A | 108.38 | C2—C3—H3C | 109.47 |
C2—C1—H1B | 108.38 | H3A—C3—H3C | 109.5 |
P1—C1—H1B | 108.38 | H3B—C3—H3C | 109.5 |
H1A—C1—H1B | 107.4 | C1—P1—C1i | 108.84 (5) |
C3—C2—C1 | 110.89 (15) | C1—P1—P2 | 110.10 (5) |
C3—C2—H2A | 109.46 | S1—P2—S1i | 112.2 (2) |
C1—C2—H2A | 109.46 | S1i—P2—Cl1 | 113.9 (8) |
C3—C2—H2B | 109.46 | S1—P2—Cl1i | 114.8 (8) |
C1—C2—H2B | 109.46 | Cl1—P2—Cl1i | 116.1 (3) |
H2A—C2—H2B | 108.0 | S1—P2—P1 | 106.6 (2) |
C2—C3—H3A | 109.47 | Cl1—P2—P1 | 101.6 (4) |
P1—C1—C2—C3 | −177.62 (13) | C1—P1—P2—S1 | −29.4 (3) |
C2—C1—P1—C1ii | 172.64 (10) | C1i—P1—P2—S1 | −149.4 (3) |
C2—C1—P1—C1i | 54.2 (2) | C1—P1—P2—Cl1ii | −148.9 (6) |
C2—C1—P1—P2 | −66.60 (13) | C1ii—P1—P2—Cl1 | 91.1 (6) |
C1ii—P1—P2—S1 | 90.6 (3) | C1—P1—P2—Cl1 | −28.9 (6) |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z. |
C9H21BrP2S2 | Dx = 1.440 Mg m−3 |
Mr = 335.23 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3c1 | Cell parameters from 1524 reflections |
a = 11.522 (3) Å | θ = 2.5–25.0° |
c = 13.450 (4) Å | µ = 3.10 mm−1 |
V = 1546.3 (7) Å3 | T = 180 K |
Z = 4 | Trigonal prism, colourless |
F(000) = 688 | 0.16 × 0.15 × 0.12 mm |
Stoe IPDS diffractometer | 1024 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 722 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.109 |
Detector resolution: 6.667 pixels mm-1 | θmax = 26.2°, θmin = 3.0° |
φ scans | h = −14→13 |
Absorption correction: numerical (XRED; Stoe & Cie, 1996) | k = −14→14 |
Tmin = 0.637, Tmax = 0.707 | l = −16→16 |
9325 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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.061 | H-atom parameters constrained |
S = 0.89 | w = 1/[σ2(Fo2) + (0.0275P)2] where P = (Fo2 + 2Fc2)/3 |
1024 reflections | (Δ/σ)max = 0.004 |
47 parameters | Δρmax = 0.36 e Å−3 |
2 restraints | Δρmin = −0.45 e Å−3 |
Experimental. Recrystallized from acetonitrile/benzene (1/10). During data collection the crystal was in cold N2 gas of the Cryostream Cooler (Oxford Cryosystems, 1992) mounted on a φ-axis diffractometer supplied with an area detector. Data collection: φ-scans, φ-incr.=1.32 °, 153 exposures |
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) | |
C1 | 0.5032 (2) | 0.2921 (3) | 0.34476 (17) | 0.0220 (6) | |
H1A | 0.5092 | 0.3071 | 0.4175 | 0.026* | |
H1B | 0.4790 | 0.3556 | 0.3146 | 0.026* | |
C2 | 0.3902 (3) | 0.1508 (3) | 0.3245 (2) | 0.0303 (7) | |
H2A | 0.3776 | 0.1365 | 0.2519 | 0.036* | |
H2B | 0.4145 | 0.0857 | 0.3514 | 0.036* | |
C3 | 0.2601 (3) | 0.1258 (3) | 0.3715 (2) | 0.0467 (9) | |
H3A | 0.1891 | 0.0342 | 0.3566 | 0.056* | |
H3B | 0.2356 | 0.1896 | 0.3446 | 0.056* | |
H3C | 0.2717 | 0.1374 | 0.4437 | 0.056* | |
Br1 | 0.5228 (15) | 0.3905 (19) | 0.0984 (13) | 0.0302 (6) | 0.3333 |
P1 | 0.6667 | 0.3333 | 0.29992 (8) | 0.0186 (3) | |
P2 | 0.6667 | 0.3333 | 0.13609 (8) | 0.0353 (4) | |
S1 | 0.5355 (19) | 0.385 (2) | 0.0973 (17) | 0.0302 (6) | 0.6667 |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0229 (15) | 0.0293 (16) | 0.0154 (11) | 0.0142 (13) | 0.0006 (10) | −0.0017 (11) |
C2 | 0.0252 (16) | 0.0283 (17) | 0.0345 (15) | 0.0113 (15) | 0.0041 (12) | −0.0018 (12) |
C3 | 0.0306 (19) | 0.044 (2) | 0.055 (2) | 0.0107 (18) | 0.0074 (15) | −0.0023 (16) |
Br1 | 0.036 (2) | 0.0513 (12) | 0.0217 (4) | 0.0352 (11) | −0.0026 (13) | −0.0006 (6) |
P1 | 0.0218 (4) | 0.0218 (4) | 0.0123 (5) | 0.0109 (2) | 0.000 | 0.000 |
P2 | 0.0473 (6) | 0.0473 (6) | 0.0114 (6) | 0.0237 (3) | 0.000 | 0.000 |
S1 | 0.036 (2) | 0.0513 (12) | 0.0217 (4) | 0.0352 (11) | −0.0026 (13) | −0.0006 (6) |
C1—C2 | 1.517 (4) | C3—H3A | 0.9800 |
C1—P1 | 1.801 (2) | C3—H3B | 0.9800 |
C1—H1A | 0.9900 | C3—H3C | 0.9800 |
C1—H1B | 0.9900 | Br1—P2 | 2.128 (6) |
C2—C3 | 1.515 (4) | P1—P2 | 2.2035 (16) |
C2—H2A | 0.9900 | P2—S1 | 1.954 (8) |
C2—H2B | 0.9900 | ||
C2—C1—P1 | 116.49 (18) | C2—C3—H3B | 109.5 |
C2—C1—H1A | 108.2 | H3A—C3—H3B | 109.5 |
P1—C1—H1A | 108.2 | C2—C3—H3C | 109.5 |
C2—C1—H1B | 108.2 | H3A—C3—H3C | 109.5 |
P1—C1—H1B | 108.2 | H3B—C3—H3C | 109.5 |
H1A—C1—H1B | 107.3 | C1i—P1—C1 | 109.38 (8) |
C3—C2—C1 | 111.4 (2) | C1—P1—P2 | 109.57 (8) |
C3—C2—H2A | 109.3 | S1i—P2—S1 | 113.1 (6) |
C1—C2—H2A | 109.3 | S1—P2—Br1i | 113.8 (12) |
C3—C2—H2B | 109.3 | S1i—P2—Br1 | 113.9 (12) |
C1—C2—H2B | 109.3 | Br1i—P2—Br1 | 114.5 (4) |
H2A—C2—H2B | 108.0 | S1—P2—P1 | 105.5 (7) |
C2—C3—H3A | 109.5 | Br1—P2—P1 | 103.8 (5) |
P1—C1—C2—C3 | 176.3 (2) | C1—P1—P2—S1i | −90.0 (8) |
C2—C1—P1—C1i | −53.0 (3) | C1—P1—P2—S1 | 30.0 (8) |
C2—C1—P1—C1ii | −172.82 (16) | C1—P1—P2—Br1i | −90.0 (5) |
C2—C1—P1—P2 | 67.1 (2) | C1i—P1—P2—Br1 | 150.0 (5) |
C1ii—P1—P2—S1i | 150.0 (8) | C1—P1—P2—Br1 | 30.0 (5) |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z. |
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