Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801008273/ya6026sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801008273/ya6026Isup2.hkl |
CCDC reference: 170284
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.011 Å
- R factor = 0.031
- wR factor = 0.079
- Data-to-parameter ratio = 18.5
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.344 0.625 Tmin and Tmax expected: 0.221 0.450 RR = 1.119 Please check that your absorption correction is appropriate. PLAT_213 Alert C Atom C10 has ADP max/min Ratio ........... 3.20 General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.720 Tmax scaled 0.450 Tmin scaled 0.248 REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 2200 Count of symmetry unique reflns 1336 Completeness (_total/calc) 164.67% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 864 Fraction of Friedel pairs measured 0.647 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998); cell refinement: DENZO and COLLECT; data reduction: DENZO and COLLECT; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
(C4H12N)[PbCl2(C6H5)3] | F(000) = 564 |
Mr = 583.54 | Dx = 1.777 Mg m−3 |
Monoclinic, I2 | Mo Kα radiation, λ = 0.71073 Å |
a = 10.3759 (3) Å | Cell parameters from 3028 reflections |
b = 9.7074 (3) Å | θ = 2.9–27.5° |
c = 10.8400 (3) Å | µ = 7.98 mm−1 |
β = 92.432 (1)° | T = 100 K |
V = 1090.85 (6) Å3 | Block, red |
Z = 2 | 0.20 × 0.20 × 0.10 mm |
Enraf Nonius KappaCCD area-detector diffractometer | 2200 independent reflections |
Radiation source: Enraf Nonius FR591 rotating-anode | 2198 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
Detector resolution: 9.091 pixels mm-1 | θmax = 27.5°, θmin = 3.8° |
φ and ω scans to fill the Ewald sphere | h = −13→13 |
Absorption correction: multi-scan (SORTAV; Blessing, 1995, 1997) | k = −11→12 |
Tmin = 0.344, Tmax = 0.625 | l = −14→13 |
3885 measured reflections |
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-atom parameters constrained |
wR(F2) = 0.079 | w = 1/[σ2(Fo2) + (0.0524P)2 + 2.6404P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max < 0.001 |
2200 reflections | Δρmax = 3.21 e Å−3 |
119 parameters | Δρmin = −4.68 e Å−3 |
1 restraint | Absolute structure: (Flack, 1983). 884 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.022 (12) |
Experimental. Lattice absences excluded from the. hkl file at the time of its creation. |
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. All non-H refined anisotropically except C4 which was refined isotropically to suppress persistent non-positive definite behaviour subsequent to the placement of H4. H in calculated positions and refined with a riding model. |
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.5000 | 0.4964 | 0.5000 | 0.00950 (11) | |
Cl1 | 0.25618 (13) | 0.5062 (5) | 0.39506 (13) | 0.0136 (4) | |
C1 | 0.5000 | 0.2682 (10) | 0.5000 | 0.0100 (18) | |
C2 | 0.5743 (7) | 0.1958 (8) | 0.5884 (6) | 0.0129 (13) | |
H2 | 0.6264 | 0.2445 | 0.6480 | 0.015* | |
C3 | 0.5724 (7) | 0.0536 (9) | 0.5895 (7) | 0.0153 (14) | |
H3 | 0.6207 | 0.0046 | 0.6517 | 0.018* | |
C4 | 0.5000 | −0.0179 (16) | 0.5000 | 0.017 (2)* | |
H4 | 0.5000 | −0.1157 | 0.5000 | 0.020* | |
C5 | 0.5661 (7) | 0.6038 (8) | 0.3354 (6) | 0.0123 (13) | |
C6 | 0.4918 (7) | 0.7061 (7) | 0.2786 (6) | 0.0115 (13) | |
H6 | 0.4112 | 0.7311 | 0.3106 | 0.014* | |
C7 | 0.5365 (8) | 0.7731 (8) | 0.1727 (7) | 0.0161 (15) | |
H7 | 0.4879 | 0.8460 | 0.1353 | 0.019* | |
C8 | 0.6510 (8) | 0.7322 (9) | 0.1240 (7) | 0.0165 (15) | |
H8 | 0.6805 | 0.7761 | 0.0521 | 0.020* | |
C9 | 0.7239 (7) | 0.6265 (9) | 0.1798 (7) | 0.0155 (15) | |
H9 | 0.8023 | 0.5984 | 0.1452 | 0.019* | |
C10 | 0.6826 (7) | 0.5625 (8) | 0.2855 (6) | 0.0123 (13) | |
H10 | 0.7327 | 0.4913 | 0.3238 | 0.015* | |
N1 | 0.0000 | 0.8165 (10) | 0.5000 | 0.0175 (18) | |
C11 | 0.0687 (10) | 0.7292 (11) | 0.5931 (8) | 0.029 (2) | |
H11A | 0.0064 | 0.6715 | 0.6347 | 0.043* | |
H11B | 0.1145 | 0.7879 | 0.6541 | 0.043* | |
H11C | 0.1308 | 0.6704 | 0.5524 | 0.043* | |
C12 | 0.0927 (11) | 0.9040 (11) | 0.4348 (9) | 0.037 (2) | |
H12A | 0.1536 | 0.8452 | 0.3925 | 0.055* | |
H12B | 0.1401 | 0.9626 | 0.4948 | 0.055* | |
H12C | 0.0457 | 0.9620 | 0.3742 | 0.055* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.00869 (14) | 0.01444 (16) | 0.00520 (14) | 0.000 | −0.00173 (9) | 0.000 |
Cl1 | 0.0087 (5) | 0.0218 (11) | 0.0100 (6) | 0.0006 (13) | −0.0047 (4) | 0.0023 (14) |
C1 | 0.013 (4) | 0.012 (5) | 0.005 (4) | 0.000 | −0.001 (3) | 0.000 |
C2 | 0.012 (3) | 0.016 (4) | 0.011 (3) | 0.001 (3) | −0.001 (2) | −0.001 (3) |
C3 | 0.012 (3) | 0.024 (3) | 0.009 (3) | 0.003 (3) | −0.003 (3) | 0.007 (3) |
C5 | 0.013 (3) | 0.018 (4) | 0.006 (3) | −0.004 (3) | −0.002 (2) | −0.003 (2) |
C6 | 0.016 (3) | 0.008 (3) | 0.010 (3) | 0.001 (3) | 0.000 (3) | 0.001 (2) |
C7 | 0.021 (4) | 0.014 (4) | 0.012 (4) | −0.002 (3) | −0.007 (3) | 0.004 (3) |
C8 | 0.017 (4) | 0.026 (4) | 0.006 (3) | −0.007 (3) | −0.002 (3) | 0.003 (3) |
C9 | 0.010 (3) | 0.027 (4) | 0.009 (3) | −0.004 (3) | −0.002 (3) | −0.005 (3) |
C10 | 0.012 (3) | 0.015 (3) | 0.009 (3) | −0.003 (3) | −0.008 (3) | 0.000 (3) |
N1 | 0.020 (4) | 0.018 (5) | 0.013 (4) | 0.000 | −0.008 (3) | 0.000 |
C11 | 0.036 (5) | 0.038 (5) | 0.011 (4) | 0.021 (4) | −0.006 (4) | 0.004 (4) |
C12 | 0.045 (6) | 0.033 (5) | 0.031 (5) | −0.024 (5) | −0.009 (4) | 0.004 (4) |
Pb1—C5i | 2.201 (7) | C7—C8 | 1.378 (12) |
Pb1—C5 | 2.201 (7) | C7—H7 | 0.9500 |
Pb1—C1 | 2.215 (10) | C8—C9 | 1.397 (12) |
Pb1—Cl1i | 2.7312 (14) | C8—H8 | 0.9500 |
Pb1—Cl1 | 2.7312 (14) | C9—C10 | 1.388 (10) |
C1—C2i | 1.394 (9) | C9—H9 | 0.9500 |
C1—C2 | 1.394 (9) | C10—H10 | 0.9500 |
C2—C3 | 1.381 (12) | N1—C11ii | 1.478 (10) |
C2—H2 | 0.9500 | N1—C11 | 1.478 (10) |
C3—C4 | 1.387 (11) | N1—C12 | 1.485 (11) |
C3—H3 | 0.9500 | N1—C12ii | 1.485 (11) |
C4—C3i | 1.387 (11) | C11—H11A | 0.9800 |
C4—H4 | 0.9500 | C11—H11B | 0.9800 |
C5—C6 | 1.386 (10) | C11—H11C | 0.9800 |
C5—C10 | 1.403 (10) | C12—H12A | 0.9800 |
C6—C7 | 1.415 (10) | C12—H12B | 0.9800 |
C6—H6 | 0.9500 | C12—H12C | 0.9800 |
C5i—Pb1—C5 | 123.5 (4) | C8—C7—H7 | 120.1 |
C5i—Pb1—C1 | 118.27 (19) | C6—C7—H7 | 120.1 |
C5—Pb1—C1 | 118.27 (19) | C7—C8—C9 | 120.4 (7) |
C5i—Pb1—Cl1i | 87.8 (2) | C7—C8—H8 | 119.8 |
C5—Pb1—Cl1i | 90.3 (2) | C9—C8—H8 | 119.8 |
C1—Pb1—Cl1i | 92.01 (10) | C10—C9—C8 | 120.4 (7) |
C5i—Pb1—Cl1 | 90.3 (2) | C10—C9—H9 | 119.8 |
C5—Pb1—Cl1 | 87.8 (2) | C8—C9—H9 | 119.8 |
C1—Pb1—Cl1 | 92.01 (10) | C9—C10—C5 | 119.5 (7) |
Cl1i—Pb1—Cl1 | 176.0 (2) | C9—C10—H10 | 120.3 |
C2i—C1—C2 | 119.5 (9) | C5—C10—H10 | 120.3 |
C2i—C1—Pb1 | 120.3 (5) | C11ii—N1—C11 | 110.0 (10) |
C2—C1—Pb1 | 120.3 (5) | C11ii—N1—C12 | 107.9 (5) |
C3—C2—C1 | 120.1 (7) | C11—N1—C12 | 110.5 (6) |
C3—C2—H2 | 119.9 | C11ii—N1—C12ii | 110.5 (6) |
C1—C2—H2 | 119.9 | C11—N1—C12ii | 107.9 (5) |
C2—C3—C4 | 120.1 (8) | C12—N1—C12ii | 110.2 (11) |
C2—C3—H3 | 120.0 | N1—C11—H11A | 109.5 |
C4—C3—H3 | 120.0 | N1—C11—H11B | 109.5 |
C3—C4—C3i | 120.0 (13) | H11A—C11—H11B | 109.5 |
C3—C4—H4 | 120.0 | N1—C11—H11C | 109.5 |
C3i—C4—H4 | 120.0 | H11A—C11—H11C | 109.5 |
C6—C5—C10 | 120.4 (6) | H11B—C11—H11C | 109.5 |
C6—C5—Pb1 | 120.9 (5) | N1—C12—H12A | 109.5 |
C10—C5—Pb1 | 118.7 (5) | N1—C12—H12B | 109.5 |
C5—C6—C7 | 119.6 (7) | H12A—C12—H12B | 109.5 |
C5—C6—H6 | 120.2 | N1—C12—H12C | 109.5 |
C7—C6—H6 | 120.2 | H12A—C12—H12C | 109.5 |
C8—C7—C6 | 119.7 (7) | H12B—C12—H12C | 109.5 |
C5i—Pb1—C1—C2i | 119.5 (4) | Cl1i—Pb1—C5—C6 | −138.7 (6) |
C5—Pb1—C1—C2i | −60.5 (4) | Cl1—Pb1—C5—C6 | 37.7 (6) |
Cl1i—Pb1—C1—C2i | −151.9 (3) | C5i—Pb1—C5—C10 | 131.6 (6) |
Cl1—Pb1—C1—C2i | 28.1 (3) | C1—Pb1—C5—C10 | −48.4 (6) |
C5i—Pb1—C1—C2 | −60.5 (4) | Cl1i—Pb1—C5—C10 | 44.1 (5) |
C5—Pb1—C1—C2 | 119.5 (4) | Cl1—Pb1—C5—C10 | −139.4 (5) |
Cl1i—Pb1—C1—C2 | 28.1 (3) | C10—C5—C6—C7 | −2.7 (11) |
Cl1—Pb1—C1—C2 | −151.9 (3) | Pb1—C5—C6—C7 | −179.8 (5) |
C2i—C1—C2—C3 | −1.1 (5) | C5—C6—C7—C8 | 2.6 (11) |
Pb1—C1—C2—C3 | 178.9 (5) | C6—C7—C8—C9 | −1.0 (12) |
C1—C2—C3—C4 | 2.3 (9) | C7—C8—C9—C10 | −0.6 (12) |
C2—C3—C4—C3i | −1.1 (5) | C8—C9—C10—C5 | 0.6 (11) |
C5i—Pb1—C5—C6 | −51.2 (5) | C6—C5—C10—C9 | 1.1 (10) |
C1—Pb1—C5—C6 | 128.8 (5) | Pb1—C5—C10—C9 | 178.2 (5) |
Symmetry codes: (i) −x+1, y, −z+1; (ii) −x, y, −z+1. |
(I) (M = Pb) | (II) (M = Sn) | |
M—Cl1 | 2.7312 (14) | 2.5982 (13) |
M—C1 | 2.215 (10) | 2.144 (7) |
M—C5 | 2.201 (7) | 2.136 (4) |
Cl1—M—C1 | 92.01 (10) | 91.46 (7) |
Cl1—M—C5 | 87.8 (2) | 88.39 (14) |
Cl1—M—Cl1i | 176.0 (2) | 177.08 (9) |
Cl1—M—C5i | 90.3 (2) | 90.19 (14) |
C1—M—C5 | 118.27 (14) | 119.02 (13) |
C1—M—Cl1i | 92.01 (10) | 91.46 (7) |
C1—M—C5i | 118.27 (19) | 119.02 (13) |
C5—M—Cl1i | 90.3 (2) | 90.19 (14) |
C5—M—C5i | 123.5 (4) | 121.96 (18) |
Cl1i—M—C5i | 87.8 (2) | 88.39 (14) |
Atom designations and symmetry code [(i) 1-x, y, 1-z] are those of the structure of (I). Bond distances and angles for (II) generated by PLATON (Spek, 1990) from the CIF associated with CSD entry YUHSOJ (Ng, 1995). |