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[(CH
3)
3PH]
3[Sb
2Cl
9] experiences four phase transitions which were found by means of calorimetry, thermogravimetry and X-ray diffraction. The crystal structure was solved in the space group
P6
3/
mmc at 382 K (phase I),
Pnam at 295 K (phase II) and
Pna2
1 at 175 K (phase V). We observed an unusual increase in symmetry from the monoclinic to the orthorhombic form at the IV
V transition. The parent hexagonal high-temperature phase I consists of highly disordered [(CH
3)
3PH]
+ cations and [Sb
2Cl
9]
3− anions with an octahedral environment of Sb
III. The transition from phases I to II is associated with the ordering of [(CH
3)
3PH]
+ cations. Moreover, the successive transformations from phases I to V are related to the change in the arrangement of Cl atoms in [Sb
2Cl
9]
3− anions from the discrete `face-sharing bioctahedra' (phase I) to two corner-sharing square pyramids. A mechanism for the phase transitions is proposed. It is observed that weak C—H
Cl interactions are responsible for the structure arrangement in low-temperature phases.
Supporting information
CCDC references: 705577; 705578; 705579
For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
Crystal data top
3(C3H10P)·Cl5Sb·Cl4Sb | Dx = 1.757 Mg m−3 |
Mr = 793.79 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pna21 | Cell parameters from 54675 reflections |
a = 14.842 (3) Å | θ = 3.9–43.9° |
b = 9.3475 (19) Å | µ = 2.76 mm−1 |
c = 21.624 (4) Å | T = 175 K |
V = 3000.1 (10) Å3 | Prism, colourles |
Z = 4 | 0.25 × 0.17 × 0.17 mm |
F(000) = 1536 | |
Data collection top
Radiation source: fine-focus sealed tube | 10215 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | θmax = 43.9°, θmin = 3.9° |
Tmin = 0.56, Tmax = 0.63 | h = −17→28 |
54675 measured reflections | k = −17→17 |
16806 independent reflections | l = −36→30 |
Refinement top
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)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.061 | w = 1/[σ2(Fo2) + (0.028P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.94 | (Δ/σ)max = 0.027 |
16806 reflections | Δρmax = 1.32 e Å−3 |
275 parameters | Δρmin = −1.31 e Å−3 |
40 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 6577 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.48 (1) |
Crystal data top
3(C3H10P)·Cl5Sb·Cl4Sb | V = 3000.1 (10) Å3 |
Mr = 793.79 | Z = 4 |
Orthorhombic, Pna21 | Mo Kα radiation |
a = 14.842 (3) Å | µ = 2.76 mm−1 |
b = 9.3475 (19) Å | T = 175 K |
c = 21.624 (4) Å | 0.25 × 0.17 × 0.17 mm |
Data collection top
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | 16806 independent reflections |
Tmin = 0.56, Tmax = 0.63 | 10215 reflections with I > 2σ(I) |
54675 measured reflections | Rint = 0.041 |
Refinement top
R[F2 > 2σ(F2)] = 0.026 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.061 | Δρmax = 1.32 e Å−3 |
S = 0.94 | Δρmin = −1.31 e Å−3 |
16806 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881, 6577 Friedel pairs |
275 parameters | Absolute structure parameter: 0.48 (1) |
40 restraints | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sb1 | 0.868146 (9) | 0.502076 (12) | 0.771895 (7) | 0.02757 (3) | |
Sb2 | 0.851422 (9) | 0.492172 (11) | 0.953298 (6) | 0.02600 (3) | |
Cl1 | 0.83779 (3) | 0.71555 (5) | 0.86443 (3) | 0.03507 (10) | |
Cl3 | 0.99641 (4) | 0.39562 (6) | 0.89204 (3) | 0.04123 (12) | |
Cl2 | 0.75835 (4) | 0.32016 (6) | 0.83404 (4) | 0.05077 (15) | |
Cl12 | 0.96900 (4) | 0.68021 (6) | 0.71659 (3) | 0.03810 (11) | |
Cl11 | 0.73589 (4) | 0.59855 (5) | 0.72251 (3) | 0.03766 (11) | |
Cl13 | 0.88782 (4) | 0.33077 (6) | 0.68513 (3) | 0.04269 (13) | |
Cl22 | 0.94898 (3) | 0.65232 (5) | 1.00883 (3) | 0.03596 (10) | |
Cl21 | 0.71255 (3) | 0.59416 (6) | 1.00994 (3) | 0.03866 (11) | |
Cl23 | 0.86955 (4) | 0.31075 (6) | 1.03697 (3) | 0.03991 (12) | |
P1 | 1.03722 (4) | 0.00601 (6) | 0.87499 (3) | 0.03608 (13) | |
C11 | 1.08503 (16) | −0.1668 (3) | 0.86552 (15) | 0.0464 (5) | |
H11A | 1.1259 (19) | −0.168 (3) | 0.8331 (12) | 0.070* | |
H11B | 1.1247 (19) | −0.190 (3) | 0.9041 (11) | 0.070* | |
H11C | 1.0437 (15) | −0.241 (3) | 0.8640 (14) | 0.070* | |
C12 | 0.9754 (2) | 0.0124 (2) | 0.94499 (15) | 0.0530 (7) | |
H12A | 0.9306 | −0.0616 | 0.9449 | 0.080* | |
H12B | 0.9466 | 0.1039 | 0.9487 | 0.080* | |
H12C | 1.0156 | −0.0015 | 0.9792 | 0.080* | |
C13 | 0.9677 (3) | 0.0468 (4) | 0.81157 (17) | 0.0751 (11) | |
H13A | 0.9366 | 0.1350 | 0.8193 | 0.113* | |
H13B | 0.9247 | −0.0287 | 0.8058 | 0.113* | |
H13C | 1.0040 | 0.0562 | 0.7750 | 0.113* | |
P2 | 0.68769 (4) | 0.98294 (6) | 1.02823 (3) | 0.03452 (12) | |
C23 | 0.78894 (16) | 0.9489 (2) | 1.06940 (11) | 0.0365 (5) | |
H23B | 0.7804 (19) | 0.942 (3) | 1.1114 (11) | 0.055* | |
H23A | 0.8211 (18) | 0.869 (2) | 1.0530 (11) | 0.055* | |
H23C | 0.829 (2) | 1.034 (2) | 1.0622 (13) | 0.055* | |
C22 | 0.63161 (16) | 1.1378 (3) | 1.05551 (13) | 0.0439 (6) | |
H22A | 0.6705 | 1.2192 | 1.0512 | 0.066* | |
H22B | 0.6162 | 1.1253 | 1.0983 | 0.066* | |
H22C | 0.5777 | 1.1528 | 1.0318 | 0.066* | |
C21 | 0.7117 (2) | 0.9999 (3) | 0.94782 (14) | 0.0589 (9) | |
H21A | 0.753 (2) | 1.079 (3) | 0.9424 (18) | 0.088* | |
H21B | 0.744 (2) | 0.915 (2) | 0.9316 (17) | 0.088* | |
H21C | 0.659 (2) | 1.013 (3) | 0.929 (2) | 0.088* | |
P3 | 0.69312 (4) | 0.97587 (6) | 0.69695 (3) | 0.03122 (11) | |
C31 | 0.68749 (19) | 0.9687 (2) | 0.77891 (12) | 0.0396 (5) | |
H31C | 0.6293 (15) | 0.970 (3) | 0.7875 (17) | 0.059* | |
H31B | 0.7186 (18) | 0.887 (2) | 0.7955 (14) | 0.059* | |
H31A | 0.7196 (19) | 1.054 (2) | 0.7956 (14) | 0.059* | |
C32 | 0.64301 (19) | 1.1368 (4) | 0.66985 (16) | 0.0528 (7) | |
H32A | 0.6726 (19) | 1.213 (3) | 0.6847 (14) | 0.079* | |
H32B | 0.643 (2) | 1.135 (4) | 0.6240 (12) | 0.079* | |
H32C | 0.5803 (19) | 1.135 (3) | 0.6815 (13) | 0.079* | |
C33 | 0.80679 (18) | 0.9653 (3) | 0.67134 (13) | 0.0450 (6) | |
H33C | 0.843 (2) | 1.049 (3) | 0.6852 (13) | 0.067* | |
H33A | 0.830 (2) | 0.883 (3) | 0.6861 (13) | 0.067* | |
H33B | 0.805 (2) | 0.971 (3) | 0.6268 (11) | 0.067* | |
H3P | 0.644 (2) | 0.863 (3) | 0.6713 (15) | 0.067* | |
H2P | 0.639 (2) | 0.874 (3) | 1.0360 (14) | 0.067* | |
H1P | 1.106 (2) | 0.093 (3) | 0.8848 (13) | 0.067* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sb1 | 0.02843 (5) | 0.02350 (6) | 0.03079 (7) | 0.00097 (4) | −0.00381 (5) | −0.00124 (5) |
Sb2 | 0.02703 (5) | 0.02250 (6) | 0.02846 (7) | −0.00034 (4) | 0.00023 (5) | −0.00070 (5) |
Cl1 | 0.0389 (3) | 0.0298 (2) | 0.0366 (2) | 0.00180 (17) | −0.0044 (2) | −0.0010 (2) |
Cl3 | 0.0327 (2) | 0.0355 (2) | 0.0554 (3) | 0.00407 (19) | 0.0017 (2) | −0.0053 (2) |
Cl2 | 0.0393 (3) | 0.0317 (3) | 0.0812 (4) | −0.0079 (2) | 0.0080 (3) | −0.0043 (3) |
Cl12 | 0.0354 (2) | 0.0367 (3) | 0.0422 (3) | −0.00196 (19) | 0.0012 (2) | 0.0030 (2) |
Cl11 | 0.0377 (3) | 0.0343 (2) | 0.0410 (3) | 0.00774 (19) | −0.0101 (2) | −0.0065 (2) |
Cl13 | 0.0475 (3) | 0.0335 (3) | 0.0471 (3) | 0.0054 (2) | −0.0023 (2) | −0.0140 (2) |
Cl22 | 0.0352 (2) | 0.0303 (2) | 0.0423 (3) | −0.00344 (18) | −0.0049 (2) | −0.0030 (2) |
Cl21 | 0.0337 (2) | 0.0415 (3) | 0.0407 (3) | 0.00604 (19) | 0.0043 (2) | −0.0006 (2) |
Cl23 | 0.0501 (3) | 0.0287 (2) | 0.0409 (3) | 0.0020 (2) | 0.0034 (2) | 0.0081 (2) |
P1 | 0.0326 (3) | 0.0340 (3) | 0.0417 (4) | −0.0055 (2) | 0.0048 (2) | −0.0045 (2) |
C11 | 0.0353 (12) | 0.0482 (12) | 0.0558 (14) | 0.0106 (9) | 0.0027 (11) | −0.0111 (13) |
C12 | 0.0638 (18) | 0.0355 (12) | 0.0599 (18) | −0.0005 (10) | 0.0257 (15) | −0.0088 (11) |
C13 | 0.114 (3) | 0.0471 (16) | 0.065 (2) | 0.0119 (18) | −0.027 (2) | −0.0006 (15) |
P2 | 0.0293 (3) | 0.0334 (3) | 0.0408 (3) | 0.00089 (19) | 0.0014 (2) | −0.0095 (2) |
C23 | 0.0423 (12) | 0.0329 (11) | 0.0344 (12) | 0.0039 (9) | −0.0013 (9) | 0.0027 (9) |
C22 | 0.0410 (12) | 0.0442 (13) | 0.0464 (15) | 0.0125 (10) | 0.0037 (10) | −0.0097 (11) |
C21 | 0.0619 (17) | 0.084 (2) | 0.0309 (14) | 0.0357 (14) | −0.0109 (14) | −0.0150 (13) |
P3 | 0.0339 (3) | 0.0304 (2) | 0.0294 (3) | −0.00254 (19) | −0.0029 (2) | 0.0041 (2) |
C31 | 0.0578 (15) | 0.0313 (10) | 0.0298 (12) | 0.0008 (9) | −0.0050 (11) | 0.0005 (9) |
C32 | 0.0451 (14) | 0.0565 (16) | 0.0568 (18) | 0.0107 (11) | −0.0018 (12) | 0.0244 (14) |
C33 | 0.0419 (13) | 0.0393 (12) | 0.0537 (17) | 0.0016 (10) | 0.0066 (11) | 0.0115 (11) |
Geometric parameters (Å, º) top
Sb1—Cl11 | 2.4097 (6) | P2—C21 | 1.782 (3) |
Sb1—Cl13 | 2.4839 (7) | P2—H2P | 1.26 (3) |
Sb1—Cl12 | 2.5385 (6) | C23—H23B | 0.92 (2) |
Sb1—Cl2 | 2.7117 (7) | C23—H23A | 0.96 (2) |
Sb1—Cl1 | 2.8616 (7) | C23—H23C | 1.01 (2) |
Sb2—Cl22 | 2.4041 (6) | C22—H22A | 0.9600 |
Sb2—Cl23 | 2.4944 (7) | C22—H22B | 0.9600 |
Sb2—Cl21 | 2.5802 (6) | C22—H22C | 0.9600 |
Sb2—Cl3 | 2.6833 (7) | C21—H21A | 0.97 (3) |
Sb2—Cl1 | 2.8448 (7) | C21—H21B | 0.99 (3) |
P1—C13 | 1.758 (3) | C21—H21C | 0.88 (3) |
P1—C12 | 1.771 (3) | P3—C31 | 1.775 (3) |
P1—C11 | 1.776 (2) | P3—C33 | 1.778 (3) |
P1—H1P | 1.32 (3) | P3—C32 | 1.777 (3) |
C11—H11A | 0.93 (2) | P3—H3P | 1.40 (3) |
C11—H11B | 1.04 (2) | C31—H31C | 0.88 (2) |
C11—H11C | 0.93 (2) | C31—H31B | 0.96 (2) |
C12—H12A | 0.9600 | C31—H31A | 1.00 (2) |
C12—H12B | 0.9600 | C32—H32A | 0.89 (2) |
C12—H12C | 0.9600 | C32—H32B | 0.99 (3) |
C13—H13A | 0.9600 | C32—H32C | 0.96 (3) |
C13—H13B | 0.9600 | C33—H33C | 0.99 (2) |
C13—H13C | 0.9600 | C33—H33A | 0.90 (2) |
P2—C22 | 1.771 (2) | C33—H33B | 0.96 (2) |
P2—C23 | 1.775 (2) | | |
| | | |
Cl11—Sb1—Cl13 | 90.13 (2) | C23—P2—C21 | 109.63 (14) |
Cl11—Sb1—Cl12 | 91.50 (2) | C22—P2—H2P | 110.6 (15) |
Cl13—Sb1—Cl12 | 89.87 (2) | C23—P2—H2P | 105.7 (14) |
Cl11—Sb1—Cl2 | 87.98 (2) | C21—P2—H2P | 108.4 (14) |
Cl13—Sb1—Cl2 | 92.33 (2) | P2—C23—H23B | 113.0 (19) |
Cl12—Sb1—Cl2 | 177.74 (2) | P2—C23—H23A | 112.1 (16) |
Cl11—Sb1—Cl1 | 85.448 (19) | H23B—C23—H23A | 112 (2) |
Cl13—Sb1—Cl1 | 175.03 (2) | P2—C23—H23C | 106.3 (18) |
Cl12—Sb1—Cl1 | 87.99 (2) | H23B—C23—H23C | 107 (2) |
Cl2—Sb1—Cl1 | 89.78 (2) | H23A—C23—H23C | 105.5 (19) |
Cl22—Sb2—Cl23 | 89.77 (3) | P2—C22—H22A | 109.5 |
Cl22—Sb2—Cl21 | 90.80 (2) | P2—C22—H22B | 109.5 |
Cl23—Sb2—Cl21 | 89.60 (2) | H22A—C22—H22B | 109.5 |
Cl22—Sb2—Cl3 | 88.45 (2) | P2—C22—H22C | 109.5 |
Cl23—Sb2—Cl3 | 92.46 (2) | H22A—C22—H22C | 109.5 |
Cl21—Sb2—Cl3 | 177.807 (19) | H22B—C22—H22C | 109.5 |
Cl22—Sb2—Cl1 | 85.60 (2) | P2—C21—H21A | 108 (2) |
Cl23—Sb2—Cl1 | 175.28 (2) | P2—C21—H21B | 112 (2) |
Cl21—Sb2—Cl1 | 89.58 (2) | H21A—C21—H21B | 105 (3) |
Cl3—Sb2—Cl1 | 88.31 (2) | P2—C21—H21C | 106 (3) |
Sb2—Cl1—Sb1 | 87.10 (2) | H21A—C21—H21C | 113 (3) |
C13—P1—C12 | 110.84 (19) | H21B—C21—H21C | 112 (3) |
C13—P1—C11 | 109.98 (16) | C31—P3—C32 | 109.97 (14) |
C12—P1—C11 | 109.65 (13) | C31—P3—C33 | 110.69 (14) |
C13—P1—H1P | 116.4 (13) | C32—P3—C33 | 109.95 (13) |
C12—P1—H1P | 104.0 (13) | C31—P3—H3P | 110.1 (14) |
C11—P1—H1P | 105.6 (13) | C32—P3—H3P | 107.0 (14) |
P1—C11—H11A | 110.8 (19) | C33—P3—H3P | 109.1 (13) |
P1—C11—H11B | 108.7 (17) | P3—C31—H31C | 105 (2) |
H11A—C11—H11B | 103.5 (19) | P3—C31—H31B | 112.2 (18) |
P1—C11—H11C | 114.9 (18) | H31C—C31—H31B | 114 (2) |
H11A—C11—H11C | 114 (2) | P3—C31—H31A | 108.0 (17) |
H11B—C11—H11C | 104 (2) | H31C—C31—H31A | 112 (2) |
P1—C12—H12A | 109.5 | H31B—C31—H31A | 106 (2) |
P1—C12—H12B | 109.5 | P3—C32—H32A | 110 (2) |
H12A—C12—H12B | 109.5 | P3—C32—H32B | 108 (2) |
P1—C12—H12C | 109.5 | H32A—C32—H32B | 112 (3) |
H12A—C12—H12C | 109.5 | P3—C32—H32C | 108 (2) |
H12B—C12—H12C | 109.5 | H32A—C32—H32C | 113 (2) |
P1—C13—H13A | 109.5 | H32B—C32—H32C | 105 (2) |
P1—C13—H13B | 109.5 | P3—C33—H33C | 112 (2) |
H13A—C13—H13B | 109.5 | P3—C33—H33A | 107 (2) |
P1—C13—H13C | 109.5 | H33C—C33—H33A | 111 (2) |
H13A—C13—H13C | 109.5 | P3—C33—H33B | 107 (2) |
H13B—C13—H13C | 109.5 | H33C—C33—H33B | 105 (2) |
C22—P2—C23 | 112.17 (12) | H33A—C33—H33B | 114 (2) |
C22—P2—C21 | 110.27 (13) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C31—H31B···Cl1 | 0.96 (2) | 2.81 (2) | 3.741 (3) | 162 (2) |
C21—H21B···Cl1 | 0.99 (3) | 2.74 (3) | 3.717 (3) | 168 (3) |
C31—H31A···Cl2i | 1.00 (2) | 2.69 (2) | 3.650 (3) | 163 (2) |
C33—H33C···Cl13i | 0.99 (2) | 2.72 (3) | 3.634 (3) | 154 (2) |
C33—H33B···Cl21ii | 0.96 (2) | 2.79 (3) | 3.703 (3) | 159 (2) |
C23—H23B···Cl11iii | 0.92 (2) | 2.82 (2) | 3.613 (3) | 145 (2) |
C23—H23C···Cl23i | 1.01 (2) | 2.71 (2) | 3.656 (2) | 157 (3) |
C21—H21C···Cl3iv | 0.88 (3) | 2.69 (3) | 3.552 (3) | 167 (3) |
C11—H11B···Cl21v | 1.04 (2) | 2.78 (2) | 3.714 (3) | 149 (2) |
P3—H3P···Cl12iv | 1.40 (3) | 2.81 (3) | 3.6571 (10) | 117 (2) |
P1—H1P···Cl2v | 1.32 (3) | 2.64 (3) | 3.7679 (11) | 142 (2) |
Symmetry codes: (i) x, y+1, z; (ii) −x+3/2, y+1/2, z−1/2; (iii) −x+3/2, y+1/2, z+1/2; (iv) x−1/2, −y+3/2, z; (v) x+1/2, −y+1/2, z. |
Crystal data top
3(C3H10P)·Cl9Sb2 | Dx = 1.709 Mg m−3 |
Mr = 793.81 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pnam | Cell parameters from 4162 reflections |
a = 15.070 (3) Å | θ = 3.2–29.4° |
b = 9.3026 (19) Å | µ = 2.68 mm−1 |
c = 22.008 (4) Å | T = 295 K |
V = 3085.3 (11) Å3 | Prism, colourles |
Z = 4 | 0.25 × 0.17 × 0.17 mm |
F(000) = 1536 | |
Data collection top
Radiation source: fine-focus sealed tube | 2130 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | θmax = 29.4°, θmin = 3.2° |
Tmin = 0.58, Tmax = 0.64 | h = −20→20 |
36684 measured reflections | k = −12→12 |
4156 independent reflections | l = −29→29 |
Refinement top
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)] = 0.031 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.107 | w = 1/[σ2(Fo2) + (0.0347P)2 + 1.255P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.002 |
4156 reflections | Δρmax = 0.56 e Å−3 |
129 parameters | Δρmin = −0.54 e Å−3 |
6 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0023 (2) |
Crystal data top
3(C3H10P)·Cl9Sb2 | V = 3085.3 (11) Å3 |
Mr = 793.81 | Z = 4 |
Orthorhombic, Pnam | Mo Kα radiation |
a = 15.070 (3) Å | µ = 2.68 mm−1 |
b = 9.3026 (19) Å | T = 295 K |
c = 22.008 (4) Å | 0.25 × 0.17 × 0.17 mm |
Data collection top
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | 4156 independent reflections |
Tmin = 0.58, Tmax = 0.64 | 2130 reflections with I > 2σ(I) |
36684 measured reflections | Rint = 0.037 |
Refinement top
R[F2 > 2σ(F2)] = 0.031 | 6 restraints |
wR(F2) = 0.107 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.56 e Å−3 |
4156 reflections | Δρmin = −0.54 e Å−3 |
129 parameters | |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sb1 | 0.651921 (19) | 0.49571 (2) | 0.838482 (12) | 0.05549 (13) | |
Cl1 | 0.68062 (12) | 0.27704 (17) | 0.7500 | 0.0771 (5) | |
Cl2 | 0.74978 (16) | 0.6770 (3) | 0.77004 (14) | 0.1003 (14) | 0.50 |
Cl3 | 0.51205 (14) | 0.5815 (2) | 0.76919 (11) | 0.0854 (11) | 0.50 |
Cl11 | 0.78634 (8) | 0.41039 (14) | 0.89209 (6) | 0.0856 (4) | |
Cl12 | 0.55617 (9) | 0.32562 (14) | 0.89428 (6) | 0.0888 (4) | |
Cl13 | 0.62685 (9) | 0.67931 (14) | 0.91890 (6) | 0.0930 (4) | |
P1 | 0.97405 (14) | 0.50818 (19) | 0.7500 | 0.0855 (6) | |
C11A | 1.0553 (10) | 0.5380 (14) | 0.8054 (6) | 0.109 (4)* | 0.50 |
C11B | 1.0059 (12) | 0.5542 (17) | 0.8230 (7) | 0.126 (5)* | 0.50 |
C12 | 0.9297 (5) | 0.3298 (7) | 0.7500 | 0.086 (2) | |
P2 | 0.32392 (9) | 0.48936 (13) | 0.91547 (6) | 0.0760 (4) | |
C21 | 0.3137 (7) | 0.4896 (5) | 0.8368 (2) | 0.120 (3) | |
H21A | 0.2744 | 0.5655 | 0.8247 | 0.179* | |
H21B | 0.2902 | 0.3989 | 0.8236 | 0.179* | |
H21C | 0.3710 | 0.5045 | 0.8188 | 0.179* | |
C22 | 0.3732 (4) | 0.6475 (7) | 0.9411 (3) | 0.123 (2) | |
H22A | 0.3405 | 0.7286 | 0.9261 | 0.185* | |
H22B | 0.4332 | 0.6523 | 0.9265 | 0.185* | |
H22C | 0.3732 | 0.6487 | 0.9847 | 0.185* | |
C23 | 0.2206 (4) | 0.4606 (6) | 0.9500 (3) | 0.1004 (17) | |
H23A | 0.191 (3) | 0.377 (3) | 0.936 (2) | 0.151* | |
H23B | 0.224 (4) | 0.459 (4) | 0.9931 (8) | 0.151* | |
H23C | 0.188 (3) | 0.544 (3) | 0.938 (2) | 0.151* | |
H1P | 0.9025 | 0.6068 | 0.7500 | 0.151* | |
H2P | 0.3792 | 0.3843 | 0.9412 | 0.151* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sb1 | 0.0581 (2) | 0.04964 (18) | 0.0588 (2) | 0.00152 (13) | −0.00503 (12) | −0.00207 (12) |
Cl1 | 0.0812 (11) | 0.0598 (9) | 0.0902 (11) | 0.0069 (8) | 0.000 | 0.000 |
Cl2 | 0.0757 (14) | 0.0690 (13) | 0.156 (4) | −0.0162 (11) | 0.0032 (15) | 0.0022 (15) |
Cl3 | 0.0621 (12) | 0.0728 (13) | 0.121 (3) | 0.0037 (10) | −0.0105 (12) | 0.0055 (13) |
Cl11 | 0.0811 (8) | 0.0878 (9) | 0.0880 (8) | 0.0163 (7) | −0.0159 (7) | −0.0115 (7) |
Cl12 | 0.0861 (9) | 0.0861 (8) | 0.0941 (8) | −0.0042 (7) | 0.0042 (7) | 0.0085 (7) |
Cl13 | 0.1001 (9) | 0.0771 (8) | 0.1018 (9) | 0.0168 (7) | −0.0099 (8) | −0.0312 (7) |
P1 | 0.0755 (13) | 0.0688 (11) | 0.1122 (16) | 0.0030 (9) | 0.000 | 0.000 |
C12 | 0.087 (5) | 0.071 (4) | 0.101 (5) | −0.020 (4) | 0.000 | 0.000 |
P2 | 0.0730 (8) | 0.0811 (9) | 0.0738 (8) | 0.0073 (6) | −0.0019 (6) | −0.0121 (6) |
C21 | 0.180 (7) | 0.121 (6) | 0.058 (3) | −0.037 (4) | 0.013 (4) | −0.011 (3) |
C22 | 0.098 (4) | 0.145 (5) | 0.127 (5) | −0.029 (4) | −0.007 (4) | −0.049 (4) |
C23 | 0.109 (4) | 0.099 (4) | 0.093 (4) | −0.007 (3) | 0.007 (4) | −0.007 (3) |
Geometric parameters (Å, º) top
Sb1—Cl12 | 2.4686 (13) | C11A—C11B | 0.853 (18) |
Sb1—Cl11 | 2.4749 (13) | P2—C21 | 1.737 (5) |
Sb1—Cl13 | 2.4884 (13) | P2—C22 | 1.742 (6) |
Sb1—Cl2 | 2.699 (3) | P2—C23 | 1.753 (6) |
Sb1—Cl3 | 2.721 (2) | P2—H2P | 1.4028 |
Sb1—Cl1 | 2.8491 (12) | C21—H21A | 0.9600 |
Cl1—Sb1i | 2.8491 (12) | C21—H21B | 0.9600 |
Cl2—Cl2i | 0.882 (6) | C21—H21C | 0.9600 |
Cl3—Cl3i | 0.845 (5) | C22—H22A | 0.9600 |
P1—C11Bi | 1.730 (16) | C22—H22B | 0.9600 |
P1—C11B | 1.730 (16) | C22—H22C | 0.9600 |
P1—C11Ai | 1.749 (14) | C23—H23A | 0.95 (3) |
P1—C11A | 1.749 (14) | C23—H23B | 0.96 (3) |
P1—C12 | 1.789 (7) | C23—H23C | 0.96 (3) |
P1—H1P | 1.4164 | | |
| | | |
Cl12—Sb1—Cl11 | 92.05 (5) | C11A—P1—H1P | 115.5 |
Cl12—Sb1—Cl13 | 89.85 (5) | C12—P1—H1P | 108.4 |
Cl11—Sb1—Cl13 | 90.31 (4) | C11B—C11A—P1 | 74.6 (16) |
Cl12—Sb1—Cl2 | 175.79 (7) | C11A—C11B—P1 | 77.0 (16) |
Cl11—Sb1—Cl2 | 91.10 (7) | C21—P2—C22 | 111.0 (3) |
Cl13—Sb1—Cl2 | 92.93 (7) | C21—P2—C23 | 110.7 (4) |
Cl12—Sb1—Cl3 | 90.80 (6) | C22—P2—C23 | 111.6 (3) |
Cl11—Sb1—Cl3 | 174.36 (6) | C21—P2—H2P | 117.1 |
Cl13—Sb1—Cl3 | 94.57 (6) | C22—P2—H2P | 101.8 |
Cl2—Sb1—Cl3 | 85.83 (8) | C23—P2—H2P | 104.3 |
Cl12—Sb1—Cl1 | 88.34 (5) | P2—C21—H21A | 109.5 |
Cl11—Sb1—Cl1 | 88.43 (4) | P2—C21—H21B | 109.5 |
Cl13—Sb1—Cl1 | 177.76 (4) | H21A—C21—H21B | 109.5 |
Cl2—Sb1—Cl1 | 88.95 (7) | P2—C21—H21C | 109.5 |
Cl3—Sb1—Cl1 | 86.79 (6) | H21A—C21—H21C | 109.5 |
Sb1—Cl1—Sb1i | 86.23 (5) | H21B—C21—H21C | 109.5 |
Cl2i—Cl2—Sb1 | 123.92 (6) | P2—C22—H22A | 109.5 |
Cl3i—Cl3—Sb1 | 124.08 (5) | P2—C22—H22B | 109.5 |
C11Bi—P1—C11B | 136.4 (12) | H22A—C22—H22B | 109.5 |
C11B—P1—C11Ai | 114.4 (9) | P2—C22—H22C | 109.5 |
C11Bi—P1—C11A | 114.4 (9) | H22A—C22—H22C | 109.5 |
C11Bi—P1—C12 | 109.5 (6) | H22B—C22—H22C | 109.5 |
C11B—P1—C12 | 109.5 (6) | P2—C23—H23A | 114 (3) |
C11Ai—P1—C12 | 114.1 (5) | P2—C23—H23B | 112 (4) |
C11A—P1—C12 | 114.1 (5) | H23A—C23—H23B | 110 (3) |
C11Bi—P1—H1P | 92.9 | P2—C23—H23C | 102 (3) |
C11B—P1—H1P | 92.9 | H23A—C23—H23C | 110 (4) |
C11Ai—P1—H1P | 115.5 | H23B—C23—H23C | 108 (4) |
Symmetry code: (i) x, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C21—H21C···Cl3 | 0.96 | 2.49 | 3.447 (9) | 171 |
C21—H21B···Cl1ii | 0.96 | 2.83 | 3.719 (7) | 154 |
C21—H21A···Cl2iii | 0.96 | 2.71 | 3.566 (7) | 149 |
C23—H23C···Cl13iii | 0.96 (3) | 2.76 (2) | 3.699 (6) | 165 (4) |
C23—H23B···Cl11iv | 0.95 (1) | 2.81 (3) | 3.679 (6) | 153 (3) |
P1—H1P···Cl2 | 1.42 | 2.43 | 3.753 (3) | 153 |
P1—H1P···Cl2i | 1.42 | 2.43 | 3.753 (3) | 153 |
Symmetry codes: (i) x, y, −z+3/2; (ii) x−1/2, −y+1/2, z; (iii) x−1/2, −y+3/2, z; (iv) −x+1, −y+1, −z+2. |
Crystal data top
C18H60Cl18P6Sb4 | Dx = 1.637 Mg m−3 |
Mr = 1587.67 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63/mmc | Cell parameters from 6828 reflections |
a = 9.1910 (13) Å | θ = 2.6–26.7° |
c = 22.011 (4) Å | µ = 2.57 mm−1 |
V = 1610.3 (4) Å3 | T = 382 K |
Z = 1 | Prism, colourles |
F(000) = 768 | 0.25 × 0.17 × 0.17 mm |
Data collection top
Radiation source: fine-focus sealed tube | 312 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | θmax = 26.7°, θmin = 2.6° |
Tmin = 0.57, Tmax = 0.64 | h = −11→11 |
6828 measured reflections | k = −11→8 |
680 independent reflections | l = −12→27 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Primary atom site location: structure-invariant direct methods |
R[F2 > 2σ(F2)] = 0.053 | Secondary atom site location: difference Fourier map |
wR(F2) = 0.169 | w = 1/[σ2(Fo2) + (0.070P)2 + 2.750P] where P = (Fo2 + 2Fc2)/3 |
S = 0.99 | (Δ/σ)max = 0.015 |
680 reflections | Δρmax = 0.31 e Å−3 |
34 parameters | Δρmin = −0.43 e Å−3 |
Crystal data top
C18H60Cl18P6Sb4 | Z = 1 |
Mr = 1587.67 | Mo Kα radiation |
Hexagonal, P63/mmc | µ = 2.57 mm−1 |
a = 9.1910 (13) Å | T = 382 K |
c = 22.011 (4) Å | 0.25 × 0.17 × 0.17 mm |
V = 1610.3 (4) Å3 | |
Data collection top
Absorption correction: multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | 680 independent reflections |
Tmin = 0.57, Tmax = 0.64 | 312 reflections with I > 2σ(I) |
6828 measured reflections | Rint = 0.031 |
Refinement top
R[F2 > 2σ(F2)] = 0.053 | 34 parameters |
wR(F2) = 0.169 | 0 restraints |
S = 0.99 | Δρmax = 0.31 e Å−3 |
680 reflections | Δρmin = −0.43 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Sb1 | 0.6667 | 0.3333 | 0.16271 (4) | 0.1208 (4) | |
Cl11 | 0.4174 (5) | 0.2087 (3) | 0.0997 (2) | 0.305 (2) | |
Cl1 | 0.5294 (2) | 0.0588 (5) | 0.2500 | 0.279 (3) | |
P1 | 0.0000 | 0.0000 | 0.2500 | 0.196 (3) | |
C11 | 0.103 (3) | 0.206 (5) | 0.2740 (19) | 0.255 (18)* | 0.33 |
C12 | 0.0000 | 0.0000 | 0.166 (2) | 0.30 (3) | 0.50 |
P2 | 0.6667 | 0.3333 | −0.0872 (3) | 0.178 (2) | |
C21 | 0.7727 (12) | 0.545 (2) | −0.0614 (11) | 0.264 (10) | 0.67 |
C22 | 0.6667 | 0.3333 | −0.1635 (9) | 0.271 (17) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sb1 | 0.1203 (4) | 0.1203 (4) | 0.1219 (7) | 0.0601 (2) | 0.000 | 0.000 |
Cl11 | 0.222 (3) | 0.400 (5) | 0.235 (3) | 0.1110 (15) | −0.108 (3) | −0.0542 (13) |
Cl1 | 0.335 (6) | 0.103 (3) | 0.321 (7) | 0.0514 (13) | 0.000 | 0.000 |
P1 | 0.168 (4) | 0.168 (4) | 0.251 (9) | 0.0841 (18) | 0.000 | 0.000 |
C12 | 0.34 (5) | 0.34 (5) | 0.20 (5) | 0.17 (2) | 0.000 | 0.000 |
P2 | 0.183 (3) | 0.183 (3) | 0.168 (4) | 0.0913 (14) | 0.000 | 0.000 |
C21 | 0.280 (17) | 0.181 (16) | 0.30 (2) | 0.090 (8) | −0.038 (9) | −0.077 (18) |
C22 | 0.34 (3) | 0.34 (3) | 0.140 (17) | 0.168 (13) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
Sb1—Cl11i | 2.421 (4) | P1—C11vii | 1.72 (4) |
Sb1—Cl11 | 2.421 (4) | P1—C12v | 1.86 (5) |
Sb1—Cl11ii | 2.421 (4) | P1—C12 | 1.86 (5) |
P1—C11 | 1.72 (4) | C11—C11v | 1.05 (8) |
P1—C11iii | 1.72 (4) | P2—C22 | 1.68 (2) |
P1—C11iv | 1.72 (4) | P2—C21ii | 1.780 (19) |
P1—C11v | 1.72 (4) | P2—C21 | 1.780 (19) |
P1—C11vi | 1.72 (4) | P2—C21i | 1.780 (19) |
| | | |
Cl11i—Sb1—Cl11 | 90.44 (16) | C11v—P1—C12v | 107.8 (14) |
Cl11i—Sb1—Cl11ii | 90.44 (16) | C11vi—P1—C12v | 72.2 (14) |
Cl11—Sb1—Cl11ii | 90.44 (16) | C11vii—P1—C12v | 107.8 (14) |
C11—P1—C11iii | 123.2 (5) | C11—P1—C12 | 107.8 (14) |
C11—P1—C11iv | 111.1 (13) | C11iii—P1—C12 | 72.2 (14) |
C11iii—P1—C11v | 111.1 (13) | C11iv—P1—C12 | 107.8 (14) |
C11iv—P1—C11v | 123.2 (5) | C11v—P1—C12 | 72.2 (14) |
C11—P1—C11vi | 111.1 (13) | C11vi—P1—C12 | 107.8 (14) |
C11iii—P1—C11vi | 123.2 (5) | C11vii—P1—C12 | 72.2 (14) |
C11iv—P1—C11vi | 111.1 (13) | C12v—P1—C12 | 180.000 (2) |
C11v—P1—C11vi | 123.2 (5) | C11v—C11—P1 | 72.2 (14) |
C11—P1—C11vii | 123.2 (5) | C22—P2—C21ii | 108.6 (8) |
C11iii—P1—C11vii | 111.1 (13) | C22—P2—C21 | 108.6 (8) |
C11iv—P1—C11vii | 123.2 (5) | C21ii—P2—C21 | 110.4 (8) |
C11v—P1—C11vii | 111.1 (13) | C22—P2—C21i | 108.6 (8) |
C11—P1—C12v | 72.2 (14) | C21ii—P2—C21i | 110.4 (8) |
C11iii—P1—C12v | 107.8 (14) | C21—P2—C21i | 110.4 (8) |
C11iv—P1—C12v | 72.2 (14) | | |
Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z; (iii) −y, x−y, −z+1/2; (iv) −y, x−y, z; (v) x, y, −z+1/2; (vi) −x+y, −x, z; (vii) −x+y, −x, −z+1/2. |
Experimental details
| (175K) | (295K) | (382K) |
Crystal data |
Chemical formula | 3(C3H10P)·Cl5Sb·Cl4Sb | 3(C3H10P)·Cl9Sb2 | C18H60Cl18P6Sb4 |
Mr | 793.79 | 793.81 | 1587.67 |
Crystal system, space group | Orthorhombic, Pna21 | Orthorhombic, Pnam | Hexagonal, P63/mmc |
Temperature (K) | 175 | 295 | 382 |
a, b, c (Å) | 14.842 (3), 9.3475 (19), 21.624 (4) | 15.070 (3), 9.3026 (19), 22.008 (4) | 9.1910 (13), 9.1910 (13), 22.011 (4) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 90, 120 |
V (Å3) | 3000.1 (10) | 3085.3 (11) | 1610.3 (4) |
Z | 4 | 4 | 1 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 2.76 | 2.68 | 2.57 |
Crystal size (mm) | 0.25 × 0.17 × 0.17 | 0.25 × 0.17 × 0.17 | 0.25 × 0.17 × 0.17 |
|
Data collection |
Diffractometer | ? | ? | ? |
Absorption correction | Multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | Multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. | Multi-scan CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm. |
Tmin, Tmax | 0.56, 0.63 | 0.58, 0.64 | 0.57, 0.64 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 54675, 16806, 10215 | 36684, 4156, 2130 | 6828, 680, 312 |
Rint | 0.041 | 0.037 | 0.031 |
(sin θ/λ)max (Å−1) | 0.975 | 0.692 | 0.633 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.061, 0.94 | 0.031, 0.107, 1.04 | 0.053, 0.169, 0.99 |
No. of reflections | 16806 | 4156 | 680 |
No. of parameters | 275 | 129 | 34 |
No. of restraints | 40 | 6 | 0 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | ? |
Δρmax, Δρmin (e Å−3) | 1.32, −1.31 | 0.56, −0.54 | 0.31, −0.43 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881, 6577 Friedel pairs | ? | ? |
Absolute structure parameter | 0.48 (1) | ? | ? |
Hydrogen-bond geometry (Å, º) for (175K) top
D—H···A | D—H | H···A | D···A | D—H···A |
C31—H31B···Cl1 | 0.96 (2) | 2.81 (2) | 3.741 (3) | 162 (2) |
C21—H21B···Cl1 | 0.99 (3) | 2.74 (3) | 3.717 (3) | 168 (3) |
C31—H31A···Cl2i | 1.00 (2) | 2.69 (2) | 3.650 (3) | 163 (2) |
C33—H33C···Cl13i | 0.99 (2) | 2.72 (3) | 3.634 (3) | 154 (2) |
C33—H33B···Cl21ii | 0.96 (2) | 2.79 (3) | 3.703 (3) | 159 (2) |
C23—H23B···Cl11iii | 0.92 (2) | 2.82 (2) | 3.613 (3) | 145 (2) |
C23—H23C···Cl23i | 1.01 (2) | 2.71 (2) | 3.656 (2) | 157 (3) |
C21—H21C···Cl3iv | 0.88 (3) | 2.69 (3) | 3.552 (3) | 167 (3) |
C11—H11B···Cl21v | 1.04 (2) | 2.78 (2) | 3.714 (3) | 149 (2) |
P3—H3P···Cl12iv | 1.40 (3) | 2.81 (3) | 3.6571 (10) | 116.8 (17) |
P1—H1P···Cl2v | 1.32 (3) | 2.64 (3) | 3.7679 (11) | 141.6 (18) |
Symmetry codes: (i) x, y+1, z; (ii) −x+3/2, y+1/2, z−1/2; (iii) −x+3/2, y+1/2, z+1/2; (iv) x−1/2, −y+3/2, z; (v) x+1/2, −y+1/2, z. |
Hydrogen-bond geometry (Å, º) for (295K) top
D—H···A | D—H | H···A | D···A | D—H···A |
C21—H21C···Cl3 | 0.96 | 2.49 | 3.447 (9) | 171.3 |
C21—H21B···Cl1i | 0.96 | 2.83 | 3.719 (7) | 153.6 |
C21—H21A···Cl2ii | 0.96 | 2.71 | 3.566 (7) | 149.3 |
C23—H23C···Cl13ii | 0.96 (3) | 2.761 (16) | 3.699 (6) | 165 (4) |
C23—H23B···Cl11iii | 0.952 (14) | 2.81 (3) | 3.679 (6) | 153 (3) |
P1—H1P···Cl2 | 1.42 | 2.43 | 3.753 (3) | 153.4 |
P1—H1P···Cl2iv | 1.42 | 2.43 | 3.753 (3) | 153.4 |
Symmetry codes: (i) x−1/2, −y+1/2, z; (ii) x−1/2, −y+3/2, z; (iii) −x+1, −y+1, −z+2; (iv) x, y, −z+3/2. |
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